Title of Invention	A PROCESS FOR THE PRODUCTION OF TRICLOPYR BUTOTYL
Abstract	A process for the production of trichlopyr-butotyl where trichloro pyridinate in solvent medium is reacted with butoxy chloro acetate in presence of phase transfer catalyst at reflux temperature; and the water present in trichloro pyridinate is removed as an azeotrope; and the reaction is continued till all butoxy chloro acetate is consumed; and the solvent is first removed by distillation at atmospheric pressure; and the product trichlopyr-butotyl is then distilled under vacuum. The yield of trichlopyr-butotyl obtained is 82 % ( based on butoxy chloro acetate) with a purity of 92 %; Dated : 27 08 2003

Title of Invention

A PROCESS FOR THE PRODUCTION OF TRICLOPYR BUTOTYL

Abstract

A process for the production of trichlopyr-butotyl where trichloro pyridinate in solvent medium is reacted with butoxy chloro acetate in presence of phase transfer catalyst at reflux temperature; and the water present in trichloro pyridinate is removed as an azeotrope; and the reaction is continued till all butoxy chloro acetate is consumed; and the solvent is first removed by distillation at atmospheric pressure; and the product trichlopyr-butotyl is then distilled under vacuum. The yield of trichlopyr-butotyl obtained is 82 % ( based on butoxy chloro acetate) with a purity of 92 %; Dated : 27 08 2003

Full Text	FORM 2 THE PATENTS ACT, 1970 (39 OF 1970) PROVISIONAL / COMPLETE SPECIFICATION (See section 10) I, MR. SHALIL S SHROFF, hereby declare - (a) that I am in possession of an invention titled - A PROCESS FOR THE PRODUCTION OF TRICLOPYR BUTOTYL That my adress for service in India is as follows : MR. SHALIL S SHROFF PLOT NO. 645/646, OBEROI CHAMBERS II, 4TH & 5TH FLOOR, NEW LINK ROAD, ANDHERI (WEST), MUMBAI400 053, MAHARASHTRA, INDIA TEL. WO. 91 22 2674 7900 (30 lines) FAX NO. 91 22 2673 6193 INDIAN NATIONAL The enclosed specification (particularly) describes the nature of invention and the manner in which it is to be performed. To The Controller of Patents, The Patent Office, At MUMBAI SUMMERY OF THE INVENTION The present invention relates to a process for preparing triclopyr-butotyl corresponding to the formula The main objective of the present invention is to produce trichlopyr-butotyl in solvent phase and to get the purity of trichlopyr-butotyl of 98 % with a yield of around 82 %; and used exclusively as herbicide. 2 A process for the production of trichlopyr-butotyl wherein sodium trichloro pyridinate in solvent medium is reacted with butoxy chloro acetate in presence of phase transfer catalyst at reflux temperature; and water present in trichloro pyridinate is removed as an azeotrope; and the reaction is continued till all butoxy chloro acetate is consumed; and the solvent is first removed by distillation at atmospheric pressure; and the product trichlopyr-butotyl is then distilled under vacuum. A mixture of 1.39 parts by wt of sodium trichloro pyridinate; 9.95 parts by wt of solvent hexane and 0.55 parts by wt of catalyst triethyl benzyl ammonium chloride (TEBA) are charged into the flask; 1.0 part by wt of butoxy chloro acetate is added slowly at temperature between 65 - 67 °C and the water present in trichloro pyridinate is removed continuously as hexane-water azeotrope; After all the water is removed, the contents are cooked at temperature between 60 - 70 °C to react all butoxy chloro acetate; The reaction mass is heated and solvent hexane is distilled out first; The product triclopyr- butotyl is then distilled off under vacuum between 5-10 torr ; 3 EXAMPLE - 1 : A mixture of 1.30 parts by wt of sodium trichloro pyridinate; 9.31 parts by wt of solvent hexane and 0.51 parts by wt of catalyst tetra butyl acetyl bromide (TBAB) are charged into the flask; 1.0 part by wt of butoxy chloro acetate is added slowly at temperature between 65 - 67 °C and the water generated during reaction is removed continuously as hexane-water azeotrope; After all the water is removed, the contents are cooked at temperature between 60-70 °C to react all butoxy chloro acetate; The reaction mass is heated and solvent hexane is distilled out first; The product triclopyr-butotyl is then distilled off under vacuum between 5-10 torr ; The yield of trichlopyr-butotyl obtained is 82 % ( based on butoxy chloro acetate) with purity of 98 %; 4 EXAMPLE -2: A mixture of 1.39 parts by wt of sodium trichloro pyridinate; 9.95 parts by wt of solvent hexane and 0.55 parts by wt of catalyst triethyl benzyl ammonium chloride (TEBA) are charged into the flask; 1.0 part by wt of butoxy chloro acetate is added slowly at temperature between 65 - 67 °C and the water generated during reaction is removed continuously as hexane-water azeotrope; After all the water is removed, the contents are cooked at temperature between 60-70 °C to react all butoxy chloro acetate; The reaction mass is heated and solvent hexane is distilled out first; The product triclopyr-butotyl is distilled off under vacuum between 5-10 torr ; The yield of trichlopyr-butotyl obtained is 82 % ( based on butoxy chloro acetate) with purity of 98 %; 5 I CLAIM. 1. A process for the production of triclopyr-butotyl where in sodium trichloro pyridinate in solvent hexane medium is reacted with butoxy chloro acetate in presence of phase transfer catalyst at reflux temperature; and water present in trichloro pyridinate is removed as hexane-water azeotrope; and the solvent hexane is first removed by distillation at atmospheric pressure; and the product triclopyr-butotyl is then distilled under vacuum; 2. A process as claimed in Claim (1) where in a mixture of 1.30-1.39 parts by wt of sodium trichloro pyridinate; 9.31 - 9.95 parts by wt of solvent haxane and 0.51 - 0.55 parts by wt of catalyst (TB AB, TEB A) are reacted with 1.0 part of butoxy chloro acetate; . . . 3. A process as claimed in Claim (1) where in the phase transfer catalyst is tetra butlyl acetyl bromide (TBAB) and triethyl benzyl ammonium chloride (TEBA) 4. A process as claimed in Claim (1) where in the reaction temperature is maintained preferably between 60 - 70°C; 5. A process as claimed in Claim (1) where in the solvent hexane is distilled off preferably at atmospheric pressure; 6. A process as claimed in Claim (1) where in the product triclopyr-butotyl is distilled under vacuum preferably between 5 - 10 torr; Dated: 27 08 2003 Signed 6

Full Text

FORM 2
THE PATENTS ACT, 1970
(39 OF 1970)
PROVISIONAL / COMPLETE SPECIFICATION
(See section 10)
I, MR. SHALIL S SHROFF,
hereby declare -
(a) that I am in possession of an
invention titled - A PROCESS FOR THE PRODUCTION OF
TRICLOPYR BUTOTYL
That my adress for service in India is as follows :
MR. SHALIL S SHROFF
PLOT NO. 645/646, OBEROI CHAMBERS II, 4TH & 5TH FLOOR,
NEW LINK ROAD, ANDHERI (WEST), MUMBAI400 053,
MAHARASHTRA, INDIA
TEL. WO. 91 22 2674 7900 (30 lines)
FAX NO. 91 22 2673 6193
INDIAN NATIONAL
The enclosed specification (particularly)
describes the nature of invention and the
manner in which it is to be performed.

To
The Controller of Patents,
The Patent Office,
At MUMBAI

SUMMERY OF THE INVENTION
The present invention relates to a process for preparing
triclopyr-butotyl
corresponding to the formula

The main objective of the present invention is to produce
trichlopyr-butotyl in solvent phase and to get the purity of
trichlopyr-butotyl of 98 % with a yield of around 82 %;
and used exclusively as herbicide.
2

A process for the production of trichlopyr-butotyl wherein sodium
trichloro pyridinate in solvent medium is reacted with butoxy chloro
acetate in presence of phase transfer catalyst at reflux temperature;
and water present in trichloro pyridinate is removed as an
azeotrope; and the reaction is continued till all butoxy chloro acetate
is consumed; and the solvent is first removed by distillation at
atmospheric pressure; and the product trichlopyr-butotyl is then
distilled under vacuum.
A mixture of 1.39 parts by wt of sodium trichloro pyridinate; 9.95
parts by wt of solvent hexane and 0.55 parts by wt of catalyst triethyl
benzyl ammonium chloride (TEBA) are charged into the flask; 1.0
part by wt of butoxy chloro acetate is added slowly at temperature
between 65 - 67 °C and the water present in trichloro pyridinate is
removed continuously as hexane-water azeotrope; After all the water
is removed, the contents are cooked at temperature between 60 - 70
°C to react all butoxy chloro acetate; The reaction mass is heated
and solvent hexane is distilled out first; The product triclopyr-
butotyl is then distilled off under vacuum between 5-10 torr ;
3

EXAMPLE - 1 :
A mixture of 1.30 parts by wt of sodium trichloro pyridinate; 9.31
parts by wt of solvent hexane and 0.51 parts by wt of catalyst tetra
butyl acetyl bromide (TBAB) are charged into the flask; 1.0 part by
wt of butoxy chloro acetate is added slowly at temperature between
65 - 67 °C and the water generated during reaction is removed
continuously as hexane-water azeotrope; After all the water is
removed, the contents are cooked at temperature between
60-70 °C to react all butoxy chloro acetate; The reaction mass is
heated and solvent hexane is distilled out first; The product
triclopyr-butotyl is then distilled off under vacuum between 5-10
torr ; The yield of trichlopyr-butotyl obtained is 82 % (
based on butoxy chloro acetate) with
purity of 98 %;
4
EXAMPLE -2:
A mixture of 1.39 parts by wt of sodium trichloro pyridinate; 9.95
parts by wt of solvent hexane and 0.55 parts by wt of catalyst triethyl
benzyl ammonium chloride (TEBA) are charged into the flask; 1.0
part by wt of butoxy chloro acetate is added slowly at temperature
between 65 - 67 °C and the water generated during reaction is
removed continuously as hexane-water azeotrope; After all the
water is removed, the contents are cooked at temperature between
60-70 °C to react all butoxy chloro acetate; The reaction mass is
heated and solvent hexane is distilled out first; The product
triclopyr-butotyl is distilled off under vacuum between 5-10 torr ;
The yield of trichlopyr-butotyl obtained is 82 % ( based on butoxy
chloro acetate) with
purity of 98 %;
5

I CLAIM.
1. A process for the production of triclopyr-butotyl where in
sodium trichloro pyridinate in solvent hexane medium is reacted
with butoxy chloro acetate in presence of phase transfer catalyst at
reflux temperature; and water present in trichloro pyridinate is
removed as hexane-water azeotrope; and the solvent hexane is
first removed by distillation at atmospheric pressure; and the
product triclopyr-butotyl is then distilled under vacuum;
2. A process as claimed in Claim (1) where in a mixture of
1.30-1.39 parts by wt of sodium trichloro pyridinate; 9.31 - 9.95
parts by wt of solvent haxane and 0.51 - 0.55 parts by wt of
catalyst (TB AB, TEB A) are reacted with 1.0 part of butoxy chloro
acetate; . . .
3. A process as claimed in Claim (1) where in the phase
transfer catalyst is tetra butlyl acetyl bromide (TBAB) and
triethyl benzyl ammonium chloride (TEBA)
4. A process as claimed in Claim (1) where in the reaction
temperature is maintained preferably between 60 - 70°C;
5. A process as claimed in Claim (1) where in the solvent
hexane is distilled off preferably at atmospheric pressure;
6. A process as claimed in Claim (1) where in the product
triclopyr-butotyl is distilled under vacuum preferably between 5 -
10 torr;

Dated: 27 08 2003 Signed
6

Documents:

852-mum-2003-abstract(27-8-2003).doc

852-mum-2003-abstract(27-8-2003).pdf

852-mum-2003-abstract(amended)-(12-2-2004).pdf

852-mum-2003-abstract(granted)-(8-12-2005).doc

852-mum-2003-abstract(granted)-(8-12-2005).pdf

852-mum-2003-cancelled pages(12-2-2004).pdf

852-mum-2003-claims(27-8-2003).doc

852-mum-2003-claims(27-8-2003).pdf

852-mum-2003-claims(amended)-(12-2-2004).pdf

852-mum-2003-claims(granted)-(8-12-2005).doc

852-mum-2003-claims(granted)-(8-12-2005).pdf

852-mum-2003-correspondence(12-2-2004).pdf

852-mum-2003-correspondence(ipo)-(28-12-2005).pdf

852-mum-2003-description(complete)-(27-8-2003).pdf

852-mum-2003-description(granted)-(8-12-2005).pdf

852-mum-2003-form 1(27-8-2003).pdf

852-mum-2003-form 1(29-9-2005).pdf

852-mum-2003-form 13(29-9-2004).pdf

852-mum-2003-form 19(29-9-2005).pdf

852-mum-2003-form 19(8-9-2003).pdf

852-mum-2003-form 2(27-8-2003).doc

852-mum-2003-form 2(27-8-2003).pdf

852-mum-2003-form 2(granted)-(8-12-2005).doc

852-mum-2003-form 2(granted)-(8-12-2005).pdf

852-mum-2003-form 2(title page)-(27-8-2003).pdf

852-mum-2003-form 2(title page)-(granted)-(8-12-2005).pdf

852-mum-2003-form 3(27-8-2003).pdf

852-mum-2003-form 3(29-9-2005).pdf

852-mum-2003-specification(amended)-(12-2-2004).pdf

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Patent Number

197707

Indian Patent Application Number

852/MUM/2003

PG Journal Number

31/2010

Publication Date

30-Jul-2010

Grant Date

Date of Filing

27-Aug-2005

Name of Patentee

SHALIL S SHROFF

Applicant Address

PLOT NO.645/646,OBEROI CHAMBERS II, 4TH & 5TH FLOOR, NEW LINK ROAD, ANDHERI(WEST), MUMBAI 400053, MAHARASHTRA, INDIA

Inventors:

#	Inventor's Name	Inventor's Address
1	SHALIL S SHROFF	PLOT NO.645/646,OBEROI CHAMBERS II, 4TH & 5TH FLOOR, NEW LINK ROAD, ANDHERI(WEST), MUMBAI 400053, MAHARASHTRA, INDIA

PCT International Classification Number

C07D213/02

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA