Title of Invention

A PROCESS FOR THE PREAPARATION OF LACTAM MACROMONOMER

Abstract This invention relates to a process for the preparation of a lactam macromonomer. The process is for the preparation of reactive prepolymers bearing a lactam functionality, capable of undergoing ring opening polymerization, and more particularly, to a process wherein the cyclic functional group is attached to a hydrophilic or hydrophobic polymer chain, as mentioned in formula (I). Wherein, R = an alkyl group with 1 -40 carbon atoms R1 - hydrogen or methyl R2 = alkylene units with 1-5 carbon atoms X = bifunctional moiety derived from mercaptoacetic acid, 3-mercaptopropionic acid, mercaptosuccinic acid, n = 3-45 m = > 2 methylene units attached to the hetero atom The Compound having the formula (I) is produced by direct esterification reaction of a carboxylic group containing polymer with a lactam with at least one active hydrogen capable reacting with the acid functionalized hydrophobic or hydrophilic prepolymer.
Full Text This present invention particularly relates to a process for the preparation of a lactam macromonomer, and more particularly to a process for the preparation of reactive prepolymers bearing a lactam functionality, capable of undergoing ring opening polymerization, and more particularly, to a process wherein the cyclic functional group is attached to a hydrophilic or hydrophobic polymer chain, as mentioned in formula (1).

(Formula Removed)
Wherein, R = an alkyl group with 1-40 carbon atoms
R1 = hydrogen or methyl
R2 = alkylene units with 1-5 carbon atoms
X = bifunctional moiety derived from mercaptoacetic acid, 3-mercaptopropionic acid,
mercaptosuccinic acid, n = 3-45 m = > 2 methylene units attached to the hetero atom
The Compound having the formula (I) is produced by direct esterification reaction of a carboxylic group containing polymer of formula (II) with a lactam with at least one active hydrogen capable reacting with the acid functionalized hydrophobic or hydrophilic prepolymer of formula (II).

(Formula Removed)
Macromonomers are defined as reactive oligomers. They are linear and carry reactive functional groups, preferably at either of the chain ends. They are classified as addition polymerizable and condensation polymerizable macromonomers based on the narure of the terminal functional groups. The molecular weight of macromonomer ranges from 500-50,000 and, particularly, in the range between 1000 and 25000. The synthesis of macromonomers is described in detail in the literature.[Sivaram,S., J.Scientific and Ind.Res.,56, 1, (1997) ; Gnanou,Y., Ind.J.Technol., .31 , 317, (1993); Corr.er.T., Adv.Polym.Sci., 62 , 95, (1984); Rempp.P.F., Adv.Polym.Sci., 58 , 53, (1981)]
Macromonomers are generally produced by ionic living polymerization, group transfer polymerization and free radical polymerization techniques. Of these, the radical roir.es of producing macromonomer are commercially well acceptable, as it does not require rigorous experimental conditions. Also, the number of monomers amenable to free radical polymerization is large. Macromonomers are useful in the production of tailor made graft copolymers and find application as surface active agents, compatibiJizers, adhesion promoter, organic coatings, and biomaterials.
Preparation of macromonomers with different functional groups is known in the prior art. For instance, U.S.Patent 5066759 describes a process for preparing macromonomer with

two antagonists functional groups. Herein the macromonomer is produced by the reaction between a diisocyanate and a prepolymer with carboxyl group at one end and hydroxyl or amino group at the other end. Eur. Pat. Appl. 248574 discloses a process for making hydrophilic macromonomer with carboxyl end group by using functionalized initiators. U.S. Patent 4818804 and British Patent 1096912 describes the preparation of carboxyl and hydroxyl containing macromonomers respectively, which are derived from the reaction between vinyl monomer and mercapto compounds with suitable functionality. The polycondensable macromonomer thus obtained contains one or more functional groups, which are attached to primary and secondary carbon atoms. This induces a difference in reactivity of the functional groups and limits the usage of such macromonomer in isocyanate polyaddition or polyesterification reactions. However a polycondensable macromonomer with functional groups attached to primary carbon atoms have been claimed and disclosed in our U.S.Patent 6,022,930. Macromonomers with terminal cyclic functional moiety is known in the prior art. U.S.Patent 5075389 discloses one such process of making poly (olefin) macromonomer containing p-phenyl glycidyl ether.
However, there is no description in the prior art of a macromonomer with lactam moiety, which is capable of undergoing ring opening polymerization.
It is therefore, the object of the present invention, to provide a method for making macromonomers with terminal lactam moiety.

Another object of the present invention is to prepare a hydrophobic or hydrophilic macromonomer with terminal lactam moiety capable of undergoing ring opening polymerization.
Accordingly, the present invention provides a process for the preparation of lactam macromonomer as mentioned in formula (I), which comprises; preparing carboxyl terminated prepolymer , reacting the said carboxyl terminated prepolymer, with a lactam, bearing at least one active hydrogen, in presence of a dehydrating agent at a temperature in the range of 0-15 deg.C arid separating the lactam macromonomer from the reaction mixture by conventional methods.
(Formula Removed)
Wherein, R = an alkyl group with 1-40 carbon atoms
R1 = hydrogen or methyl
R2 = alkylene units with 1-5 carbon atoms
X = bifunctional rnoiety derived from mercaptoacetic acid, 3-mercaptopropionic
acid, mercaptosuccinic acid. n = 3-45 m > 2 methylene units attached to the hetero atom

In an embodiment of (he present invention the carboxyl group containing prepolymer may be prepared by polymerizing a monomer' such as methyl methacrylate. butyl methacrylate, lauryl methacrylate, ethyl acrylate, butyl acrylate. he.xyl acrylale, n-oetyl acrylate, 2-ethylhexyl acrylate, nonyl acrylate, lauryl acrylate and styryl acrylate in presence of a bifunctional agent such as mercaptoacetic acid, 3-mercaptopropionic acid, mercaptosuccinic acid.
In another embodiment of the present invention the lactam s used may be derived from compounds containing more than or equal to 2 carbon atoms in the ring and may or may not contain other functional groups, which are exemplified by pyrrolidones, C-alkylated pyrrolidones, piperidine, butanolactam, pentanolactam, hexanolactam, dodecyllactam.
In still another embodiment of the present invention the dehydrating agent used may include, but not limited to, 1,3-dicyclohexylcarbodiimide, N,N'carbonyIdiimidazole. 1,3-dicyclohexylcarbodiirnide and aminopyridine, phenyl dichlorophosphate, chlorosulfonyl isocyanate, chlorosilanes, a mixture of alkyl chloroformate and triethyl amine, a mixture of cyanuric chloride and triethyl amine, a mixture of pyridine hydrochloride and tributylamine and a mixture of 2-chloro-l,3,5 trinitrobenzene, pyridine and phosphate ester.
In a feature of the present invention, the prepolymer containing the carboxyl group can be prepared in any conventional resin reactor equipped with a cooling jacket, a double walled condenser, a thermowell, and an addition funnel. Stirring can be done by using a

magnetic stirrer or by any stirring device. The polymerization reaction can be carried out between 40°C and 100°C and more preferably between 60°C and 90°C. The reaction is exothermic in the beginning and can be controlled by circulating cool water or by drop wise feeding of monomer. The desired molecular weight of the macromonorr.er is obtained by adjusting molar ratio of bifunctional agent to monomer. The amount in mol percentage of the bifunctional agent based on the amount of monomer chared is preferably in the range between 1 and 45. The polymerization is initiated by the addition of initiator which have a decomposition half life at 70±10°C is In yet another feature of the present invention, the macromonomer capable of undergoing ring opening polymerization is.obtained by the esterification reaction between the prepolymer and the lactam with at least one active hydrogen. The esterification reaction is carried at room temperature in the presence of a suitable carboxyl group activator (CGA). The reaction is carried out by mixing the prepolymer in a suitable solvent- The prepolymer solution is preferably cooled between 0°C to 15°C followed by addit:on of lactam and the dehydrating agent. Alternatively, the prepolymer solution can aho be added to a cooled mixture of lactam and the dehydrating agent. The urea formed caring

the reaction if filtered off and the luctam mncromonomer is recovered by distilling the solvent.
The process for the present invention is described herein below with examples that are illustrative only and should not be construed to limit the scope of the present invention in any manner.
Example 1;
In a three neck 100 mL round bottom flask fitted with a thermowell, condenser, a magnetic needle and a glass tube for nitrogen purging, was charged 25 g laurylmethacrylate, 3.6 g mercapto acetic acid, 0.16 g azobis isobutyronitrile and 29 mL toluene. The reaction mixture was stirred by means of a magnetic stirrer and purged with nitrogen gas. The flask was then heated up to 80° C. The reaction was continued till the disappearance of olifinic signals in 1H NMR spectrum. The polymer obtained is precipitated in methanol and washed thoroughly with methanol. The solvent is allowed to evaporate and the polymer is dried under vacuum at room temperature. In a separate three neck 100 mL round bottom flask fitted with a condenser, a magnetic needle and a glass tube for nitrogen purging, 2.5 g of the above prepolymer is taken and added 50 mL dry dichloromethane. The temperature of the flask is maintained at 0°C. 1.0 g 1,3-dicyclohexylcarbodiimide, 10 milligram dimethyl aminopyridine are then added followed by 0.6 g E-caprolactam. The reaction was continued for 6 hours. Urea formed during the reaction is removed by filtration and the lactam macromonomer is obtained by evaporating the filtrate. Degree of functionality, fn =0.95

Number average molecular weight, Mn = 880 Yield. %= 78
Example 2:
In a three neck 100 mL round bottom flask fitted with a theimovvell. condens?:. a magnetic needle and a glass tube for nitrogen purging, was charged 25 g laurylmethacrylate, 1.8 g mercapto acetic acid, 0.16 g azobis isobutyronitrile and 29 mL toluene. The reaction mixture was stirred by means of a magnetic stirrer and purged with nitrogen gas. The flask was then heated up to 80° C. The reaction was continued til: the disappearance of olifinic signals in 1H NMR spectrum. The polymer obtained is precipitated in methanol and washed thoroughly with methanol. The solvent is in en allowed to evaporate and the polymer is dried under vacuum at room temperature. In a separate three neck 100 mL round bottom flask fitted with a condenser, a magnetic needle and a glass tube for nitrogen purging, 5 g of the above prepolymer is taken and added 50 mL dry dichloromethane. The temperature of the flask is maintained at 0°C. 1.0 g 1,3-dicyclohexylcarbodiimide, 10 milligram dimethyl aminopyridine are then added followed by 0.6 g e-caprolactam. The reaction was continued for 6 hours. Urea formed during the reaction is removed by filtration and the lactam macromonomer is obtained by evaporating the filtrate. Degree of functionality, fn =0.95
Number average molecular weight, Mn =1910 Yield,,% = 82

Example 3:
In a three neck 100 mL round bottom flask fitted with a thcrmowell, condenser, a magnetic needle and a glass tube for nitrogen purging, was charged 25 g laurylmethacrylate, 0.73 g mercapto acetic acid, 0.16 g azobis isobutyronitrile and 29 mL toluene. The reaction mixture was stirred by means of a magnetic stirrer and purged with nitrogen gas. The flask was then heated up to 80° C. The reaction was continued till the disappearance of olifinic signals in 1H NMR spectrum. The polymer obtained is precipitated in methanol and washed thoroughly with methanol. The solvent is then allowed to evaporate and the polymer is dried under vacuum at room temperature. In a three neck 100 mL round bottom flask fitted with a condenser, a magnetic needle and a glass tube for nitrogen purging, 5.0 g of the above prepolymer is taken and added 50 mL dry dichloromethane. The temperature of the flask is maintained at 0°C. 0.5 g 1,3-dicyclohexylcarbodiimide, 5.0 milligram dimethyl aminopyridine are then added followed by 0.27 g caprolactam. The reaction was continued for 6 hours. Urea formed during the reaction is removed by filtration and the lactam macromonomer is obtained by evaporating the filtrate. Degree of functionality, fn =0.86
Number average molecular weight, Mn = 4900 Yield, % = 87
Example 4 :
In a three neck 100 mL round bottom flask fitted with a thermowcll, condenser, a magnetic needle and a glass tube for nitrogen purging, was charged 25 g methyl

methacrylute. 3.6 g inetvapto acetic acid, 0.16 g azobis isobutyronitrilc and 29 mL toluene. The reaction mixture was stirred by means of a magnetic stirrer and purged with nitrogen gas. The flask was then heated up to 80° C. The reaction was continued till the disappearance of olifinic signals in 1H NMR spectrum. The polymer obtained is precipitated in methanol and washed thoroughly with methanol. The solvent is then allowed to evaporate and the polymer is dried under vacuum at room temperature. In a three neck 100 mL round bottom flask fitted with a condenser, a magnetic needle and a glass tube for nitrogen purging, 2.5 g of the above prepolymer is taken and added 50 mL dry dichloromethane. The temperature of the flask is maintained at 0°C. 1.0 g 1,3-dicyclohexylcarbodiimide, 10 milligram dimethyl aminopyridine are then added followed by 0.6 g caprolactam. The reaction was continued for 6 hours. Urea formed during the reaction is removed by filtration and the lactam niacromonomer is obtained by evaporating the filtrate. Degree of functionality. fr =0.95
Number average molecular weight, M,, - 980 Yield, % = 78
Example 5 :
In a three neck 100 mL round bottom flask fitted with a thermowell, condenser, a magnetic needle and a glass tube for nitrogen purging, was charged 25 g methyl methacrylate, 1.8 g mercapto acetic acid, 0.16 g azobis isobutyronitrile and 29 mL toluene. The reaction mixture was stirred by means of a magnetic stirrer and purged with nitrogen gas. The flask was then heated up to 80° C. The reaction was continued till the

disappearance of olifinic signals in 1H NMR spectrum. The polymer obtained is precipitated in methanol and washed thoroughly, with methanol. The solvent is then allowed to evaporate and the polymer is dried under vacuum at room temperature. In a three neck 100 mL round bottom flask fitted with a condenser, a magnetic needle and a glass tube for nitrogen purging. 5 g of the above prepolymer is taken and added 50 mL dry dichloromethane. The temperature of the flask is maintained at 0°C. 1.0 g 1,3-dicyclohexylcarbodiimide, 10 milligram dimethyl aminopyridine are then added followed by 0.6 g caprolactam. The reaction was continued for 6 hours. Urea formed during the reaction is removed by filtration and the lactam macromonomer is obtained by evaporating the filtrate. Degree of functionality, fn =0.95
Number average molecular weight, Mn = 2080 Yield, % = 78
Example 6 :
In a three neck 100 mL round bottom flask fitted with a thermowell, condenser, a magnetic needle arid a glass tube for nitrogen purging, was charged 25 g methyl methacrylate, 0.72 g mercapto acetic acid, 0.16 g azobis isobutyronitrile and 29 mL toluene. The reaction mixture was stirred by means of a magnetic stirrer and purged with nitrogen gas. The flask was then heated up to 80° C. The reaction was continued till the disappearance of olifinic signals in 1H NMR spectrum. The polymer obtained is precipitated in methanol and washed thoroughly with methanol. The solvent is then allowed to evaporate and the polymer is dried under vacuum at room temperature. In a

throe neck 100 niL round bottom flask fitted \\ith a condenser, a magnetic needle and a glass tube for nitrogen purging, 5.0 g of the above, prepolvmer is taken and added 50 mL dry dichloromethane. The temperature of the flask is maintained at 0°C. 0.5 g 1,3-dicyclohexylcarbodiimide, 5.0 milligram dimethyl aminopyridine are then added followed by 0.27 g caprolactam. The reaction was continued for 6 hours. Urea formed during the reaction is removed by filtration and the lactam macromonomer is obtained by evaporating the filtrate. Degree of functionality, f =0.81
Number average molecular weight, Mn =4800 Yield, % = 78
Example 7:
In a three neck 100 mL round bottom flask fitted with a thermowell, condenser, a magnetic needle and a glass tube for nitrogen purging, was charged 25 g laurylmethacrylate, 21.6 g mercapto acetic acid. 0.16 g azobis isobutyronitrile and 29 mL toluene. The reaction mixture was stirred by means of a magnetic stirrer and purged with nitrogen gas. The flask was then heated up to 80° C. The reaction was continued till the disappearance of olifinic signals in !H NMR spectrum. The polymer obtained is precipitated in methanol and washed thoroughly with methanol. The solvent is allowed to evaporate and the piolymer is dried under vacuum at room temperature. In a separate three neck 100 mL round bottom flask fitted with a condenser, a magnetic needle and a glass tube for nitrogen purging, 2.5 g of the above prepolymer is taken and added 50 mL dry dichloromethane. The temperature of the flask is maintained at ()°C. 1.0 g 1,3-

dicyclohcvylcarbodiimide, 10 milligram dimethyl aminopyridinc are then added followed by 0.4 g huiryl lactnm. The reaction was continued for 6 hours. Urea formed during the reaction is removed by filtration and the lactam macromonomer is obtained by evaporating the filtrate. Degree of functionality. fr =0.72
Number average molecular weight, Mn =910 Yield, % =71
Example 8:
In a three neck 100 mL round bottom flask fitted with a thermowell, condenser, a magnetic needle and a glass tube for nitrogen purging, was charged 25 g methyl methacryiate, 3.6 g mercapio acetic acid, C.I6 g azobis isobutyroniinlc and 29mL toluene. The reaction mixture was stirred by means of a magnetic stirrer and purged with nitrogen gas. The flask was then heated up to 80° C. The reaction was continued till the disappearance of olifinic signals in 1H NMR spectrum. The polymer obtained is precipitated in methanol and washed thoroughly with methanol. The solvent is then allowed to evaporate and the polymer is dried under vacuum at room temperature. In a three neck 100 mL round bottom flask fitted with a condenser, a magnetic needle and a glass tube for nitrogen purging, 2.5 g of the above prepolymer is taken and added 50 mL dry dichloromethane. The temperature of the flask is maintained at 0°C. 1.0 g 1,3-dicyclohexylcarbodiimide, 10 milligram dimethyl aminopyridine are then added followed by 0.4 g lauryl lactam. The reaction was continued for 6 hours. Urea formed during the

reaction is removed by filtration and the lactam macromonomer is obtained by
evaporating the filtrate.
Degree of functionality, fn =0.76
Number average molecular weight, Mn= 1020 Yield, % = 81
Example9:
In a three neck 100 mL round bottom flask fitted with a thermowell, condenser, a magnetic needle and a glass tube for nitrogen purging, was charged 25 g laurylmethacrylate, 1.8 g mercapto acetic acid, 0.16 g azobis isobutyronitrile and 29 mL toluene. The reaction mixture was stirred by means of a magnetic stirrer and purged with nitrogen gas. The flask was then heated up to 80° C. The reaction was continued till the disappearance of oliifinic signals in 1H NMR spectrum. The polymer obtained is precipitated in methanol and washed thoroughly with methanol. The solvent is then allowed to evaporate and the polymer is dried under vacuum at room temperature. In a separate three neck 100 mL round bottom flask fitted with a condenser, a magnetic needle and a glass tube for nitrogen purging, 7 g of the above prepolymer is taken and added 50 mL dry dichloromethane. The temperature of the flask is maintained at 0°C. 1.8 mL ethyl chloroformate and 0,5 mL triethyl amine are then added foUrea forllowed by 1.0 g 6-caprolactam. The reaction was continued for 6 hours. The lactam macromonomer is obtained by evaporating the filtrate. Yield, % = 63
Example 10:

In a three neck 100 mL round bottom flask fitted with a thennowell, condenser, a magnetic needle and a glass tube for nitrogen purging, was charged 25 g laurylmethacrylate, 1.8 g mercapto acetic acid, 0.16 g azobis isobutyronitrile and 29 mL toluene. The reaction mixture was stirred by means of a magnetic stirrer and purged with nitrogen gas. The flask was then heated up to 30° C. The reaction was continued till the disappearance of olifinic signals in 1H NMR spectrum. The polymer obtained is* precipitated in methanol and washed thoroughly with methanol. The solvent is then allowed to evaporate and the polymer is dried under vacuum at room temperature. In a separate three neck 100 mL round bottom flask fitted with a condenser, a magnetic needle and a glass tube for nitrogen purging, 2 g of the above prepolymer is taken and added 25 mL dry dichloromethane. The temperature of the flask is maintained at 0°C. 0.8 g cyanuric chloride and 0.3 mL triethyl amine are then added followed by 0.3 g e-caprolactam. The reaction was continued for 6 hours. The lactam macromonomer is obtained by evaporating the filtrate. Yield, % = 71
Example 11:
In a three neck 100 mL round bottom flask fitted with a thermowell, condenser, a magnetic needle and a glass rube for nitrogen purging, was charged 25 g laurylmethacrylate, 1.8 g mercapto acetic acid, 0.16 g azobis isobutyronitrile and 29 mL toluene. The reaction mixture was stirred by means of a magnetic stirrer and purged with nitrogen gas. The flask was then heated up to 80° C. The reaction was continued till the disappearance of olifinic signals in 1H NMR spectrum. The polymer obtained is

gen gas. The flask was then heated up to 80° C. The reaction was continued till the disappearance of olifinic signals in 1H NMR spectrum. The polymer obtained is precipitated in methanol and washed thoroughly with mcthanol. The solvent is then allowed to evaporate and the polymer is dried under vacuum at room temperature. In a separate three neck 100 mL round bottom flask fitted with a condenser, a magnetic needle and a glass tube for nitrogen purging, 5 g of the above prepolymer is taken and added 50 mL dry dichloromethane. The temperature of the flask is maintained at 10°C. 1.0 g 1,3-dicyclohexylcarbodiimide, 10 milligram dimethyl aminopyridine are then added followed by 0.6 g e-caprolactam. The reaction was continued for 6 hours. Urea formed during the reaction is removed by filtration and the lactam macromonomer is obtained by evaporating the filtrate. Yield, % = 80
Example 12:
In a three neck 100 mL round bottom flask fitted with a thermowell, condenser, a magnetic needle and a glass tube for nitrogen purging, was charged 25 g laurylmethacrylate, 1.8 g mercapto acetic acid, 0.16 g azobis isobutyronitrile'and 29 mL toluene. The reaction mixture was stirred by means of a magnetic stirrer and purged with nitrogen gas. The flask was then heated up to 80° C. The reaction was continued till the disappearance of olifinic signals in !H NMR spectrum. The polymer obtained is precipitated in methanol and washed thoroughly with methanol. The solvent is then allowed to evaporate and the polymer is dried under vacuum at room temperature. In a

separate throe nook 100 mL round bottom flask fitted with a condenser, a magnetic noodle and a glass tube for nitrogen purging. 5 g of the above prepolymer is taken and added 50 mL dry dichloromethane. The temperature of the flask is maintained at 0CC. 1.0 g 1,3-dieyclohexylcarbodiimide, 10 milligram dimethyl aminopyridine are then added followed by 0.6 g e-caprolactam. The reaction was continued for 3 hours. Urea formed during the reaction is removed by filtration and the lactam macromonomer is obtained by evaporating the filtrate. Yield, % = 83

WE CLAIM
1. A process for the preparation of lactam macromonomer as mentioned in formula (I), which comprises; preparing carboxyl terminated prepolymer , reacting the said carboxyl terminated prepolymer, with a lactam, bearing at least one active hydrogen, in presence of a dehydrating agent at a temperature in the range of 0-15 deg.C and separating the lactam macromonomer from the reaction mixture by conventional methods.
(Formula Removed)
Wherein,
R = an alkyl group with 1-40 carbon atoms
R1 = hydrogen or methyl
R2 = alkylene units with 1-5 carbon atoms
X = bifunctional moiety derived from mercaptoacetic acid, 3-
mercaptopropionic acid, mercaptosuccinic acid. n = 3-45 m > 2 methylerie units attached to the hetero atom
2. A process as claimed in claim 1 wherein, the carboxyl terminated prepolymer is prepared by polymerizing a monomer selected from methyl methacrylate, butyl

methacrylate, lauryl methacrylate, ethyl acrylate, butyl acrylate, hexyl acrylate, n-octyl acrylate, 2-ethylhexyl acrylate, nonyl acrylate, lauryl acrylate and styryl acrylate in presence of a bifunctional agent or polymerization chain transfer agent which includes me reap to ace tic acid, 3-mercaptopropionic acid, mercaptosuccinic acid.
3. A process as claimed in claim land 2 wherein, the prepolymer has a number average molecular weight in the range between 700 and 7000.
4. A process as claimed in claims 1 to 3 wherein, the lactam s used are derived from
lactam having greater than or equal to 2 carbon atoms in the ring optionally
containing other functional groups, selected from pyrrolidones, C-alkylated
pyrrolidones, piperidine, butanolactam, pentanolactam, hexanolactam,
dodecyllactam.
5. A process as claimed in claims 1 to 4 wherein, the dehydrating agent are selected
from 1,3-dicyclohexylcarbodiimide, N,N'carbonyldiimidazole, 1,3-
dicyclohexylcarbodiimide and aminopyridine, phenyl dichlorophosphate,
chlorosulfonyl isocyanate, chlorosilanes, a mixture of alkyl chloroformate and
triethyl amine, a mixture of cyanuric chloride and triethyl amine, a mixture of
pyridine hydrochloride and tributyl amine and a mixture of 2-chloro-1,3,5-
trinitrobenzene, pyridine and phosphate ester.

6. A process for the preparation of lactam macromonomer substantially described herein with reference to examples.

Documents:

967-del-2000-abstract.pdf

967-del-2000-claims.pdf

967-del-2000-correspondence-others.pdf

967-del-2000-correspondence-po.pdf

967-del-2000-description (complete).pdf

967-del-2000-form-1.pdf

967-del-2000-form-19.pdf

967-del-2000-form-2.pdf

abstract.jpg


Patent Number 242168
Indian Patent Application Number 967/DEL/2000
PG Journal Number 34/2010
Publication Date 20-Aug-2010
Grant Date 17-Aug-2010
Date of Filing 01-Nov-2000
Name of Patentee COUNCIL OF SCIENTIFIC AND INDUSTRIAL RESEARCH
Applicant Address RAFI MARG, NEW DELHI-110001, INDIA.
Inventors:
# Inventor's Name Inventor's Address
1 LAGUDI SRINIVASAN RAMANATHAN NATIONAL CHEMICAL LABORATORY, PUNE, MAHARASTRA, INDIA.
2 SWAMINATHAN SIVARAM NATIONAL CHEMICAL LABORATORY, PUNE, MAHARASTRA, INDIA.
PCT International Classification Number C08G 61/00
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA