Title of Invention

PROCESS FOR PREPARATION OF 2-AMINO-4,6-DIMETHOXYPYRIMIDINE

Abstract

Accordingly there is provided the process for the preparation of 2- AMINO-4,6-DIMETHOXYPYRIMIDINE which comprises a process for the preparation of 2-Amino-4,6-dimethoxypyrimidine comprises, charging methanol to mixture of Toluene and Malanonitrile at room temperature in MS jacketed glass line reactor With constant stirring ; passing dry HCL gas to reaction mass of step (i in claim 1) at temperature varying from 0°C to 20°C; obtaining 3-amino-3-methoxy-N -2-cyano 2-propeimidate after constant stirring and filtration thereof; inoculating the reaction mass of step (iii in claim 1) to the solution of water, sodium bicarbonate and 50% cynamide maintained at temperatures between 0°C to 5°C;heating, stirring and filtering the reaction mass of step (iv in claim 1) to produce a slurry; reacting the slurry of step (v in claim 1) with Toluene to reflux temperature to obtain clear solution; cooling the clear solution of step (vi in claim 1) between the temperature 55°C to 63CC; adding further the activated char coal to separate unwanted impurities; transferring after filtering the reaction mass of step (viii in claim 1) into another vessel for cooling to room temperature, thereby obtaining the final product, 2-Amino-4,6-Dimethoxypyrimidine;

Full Text

FORM-2 THE PATENTS ACT, 1970 (39 OF 1970) COMPLETE SPECIFICATION (SEE SECTION 10) PROCESS FOR PREPARATION OF 2-AMINO- 4,6-DIMETHOXYPYRIMIDINE Name and address of applicants: M/s. Sajjan India Limited, Matulya Centre, #2Ground floor, Senapati Bapat Marg, Lower Parel, Mumbai400 013, Maharashtra, India, Indian. following specification particularly describes the nature of invention and the manner in which it is to be performed. (1) Field of the Invention The present invention relates to a process for preparation of 2-AMINO 4,6 DIMETHOXYPYRIMIDINE. More particularly, present invention relates to the process for production of 2 AMINO 4,6 DIMETHOXYPYRIMIDINE without emission and/or creation of any harmful effluents as it is done by purging of Chlorine gas with hydrocarbons thereby using less raw material, energy and other resources. (2) The Prior Art The preparation of 2-AMINO 4,6 DIMETHOXYPYRIMIDINE is done commercially by using one of two most popular processes namely (i) by heating of liquid.( 30% ) HCL and (ii) by use of Sodium Chloride in sulphuric acid. The process of production of 2-AMINO 4,6 DIMETHOXYPYRIMIDINE by use of anhydrous HCL has several disadvantages. The foremost disadvantage being that it requires a reactor in which 30 % HCL liquid is heated to a temperature between 140°C to 145°C under pressure thereby creating a vacuum. Another disadvantage of using this process for the preparation of 2-AMINO 4,6 DIMETHOXYPYRIMIDINE is that, during the process and also on completion of the same, effluents are generated which are not only harmful to environment but are also hazardous to life of living organisms including human beings. The other method of production of 2-AMINO 4,6 DIMETHOXYPYRIMIDINE is done by the use of Sodium Chloride, which is used by charging the same with sulphuric acid (98%). The drawback, in using and/or adopting this process for production of 2 anhydrous HCL gas is that this method causes creation of harmful and hazardous effluents which are solid and/or liquid in nature. The inorganic aqueous effluents and bye products formed by use of this process need to be neutralized prior to being discharged into the environment. In order to neutralize the effluents, separate plants are required for aqueous and solid effluents thereby increasing the cost of manufacturing and effluent treatment. Several manufacturers do not adopt these practices as treating the effluent is cost intensive process and requires additional space. However the best the effluent may be treated, none can neutralize the effluent to be absolutely free from harmful elements or compounds which are derived from the combination of HCL and Toluene. In order to free Toluene from residue water is to be added and water settlement, the Toluene is separated. The remaining aqueous effluent consists mainly of diluted liquid ( 30%) HCL and water, for neutralization. Inspite of treating the effluents and using all commercially possible processes of neutralization of the aqueous effluents, there always remains in the effluent, 0.2 % to 0.5 % of Toluene, which finds its way into the environment. Hence, it becomes extremely necessary for manufacturers to install necessary equipment to prevent pollution and to be released into the environment without having some quantities of HCL solution and other harmful bye products. In order to prevent the contamination of the environment, it becomes necessary to have harmful residue and bye products incinerated, thereby adding to the costs of manufacturing of the product and increasing use of costly natural resources, energy, and labor for 2-AMINO-4,6-DMETHOXYPYRIMIDINE . Hence, both above said popularly used methods are harmful, cost-intensive and cumbersome. 3 It is, therefore, an object of the present invention to provide a process for producing 2-AMING-4,6-DIMETHOXYPYRIMIDINE without generating any sort of effluent especially acidic, inorganic and or their variants. It is also object of the present invention to provide a method of purging the anhydrous HCL gas with a solution consisting of Toluene, Malanononitrile and Methanol. Further, it is also the object of the present invention to produce raw material of PVC compound. Still further, it is also the object of present invention to cause the production of 100% pure intermediate product of 2-AMINO-4,6-DIMETHOXYPYRIMIDINE by using less raw material, time, energy and other resources. BRIEF SUMMARY OF THE INVENTION The above and other objects of present invention are achieved by a process of purging Chlorine gas with hydrocarbons to produce anhydrous HCL gas for being utilized for the preparation of various organic molecules. The present invention provides for the production of 2-AMIN-4,6-DDVIETHOXYPYRIMID1NE commercially by purging of Chlorine gas with hydrocarbon thereby producing anhydrous HCL. It is also one of the object of the present invention to produce anhydrous HCL without creating any sort of pollutants and/or harmful effluent. 4 Another object of this invention is to provide a method for the production of 2-AMINO-4,6-DIMETHOXYPYRIMIDINE by using less raw material, energy and other resources. The novelty in the present process is the purging of chlorine gas with liquid hydrocarbons to produce anhydrous HCL gas at controlled pressure. Accordingly there is provided the process for the preparation of 2- AMINO-4,6-DMETHOXYPYRIMIDINE which comprises a process for the preparation of 2-Amino-4,6-dimethoxypyrimidine comprises, charging methanol to mixture of Toluene and Malanonitrile at room temperature in MS jacketed glass line reactor with constant stirring; passing dry HCL gas to reaction mass of step (i in claim 1) at temperature varying from 0°C to 20°C;obtaining 3-amino-3-methoxy-N - cyano 2-propeimidate after constant stirring and filtration thereof; inoculating the reaction mass of step (iii in claim 1) to the solution of water, sodium bicarbonate and 50% cynamide maintained at temperatures between 0°C to 5°C;heating, stirring and filtering the reaction mass of step (iv in claim 1) to produce a slurry; reacting the slurry of step (v in claim 1) with Toluene to reflux temperature to obtain clear solution; cooling the clear solution of step (vi in claim 1) between the temperature 55°C to 63°C; adding further the activated char coal to separate unwanted impurities; transferring after filtering the reaction mass of step (viii in claim 1) into another vessel for cooling to room temperature, thereby obtaining the final product, 2-Amino-4,6-Dimethoxypyrimidine; 5 DETAILED DESCRIPTION OF THE INVENTION The present invention now will be described more fully and particularly hereinafter. STEP I For initiating the process, a reactor consisting of MS jacketed glass line and an agitator also made of MS glass line is required. In the reactor Toluene is charged and is continuously stirred until optimum temperature is achieved between 0°C to 30°C. On reaching the optimum temperature, the same is maintained and under stirring Methanol is added to the Toluene, pursuant to which Malanonitrile is further added to the solution, while stirring of the solution continues. The temperature of the solution is then reduced to an optimum temperature ranging between 0°C to 20°C and is kept constant until the reaction is completed. The solution becomes a thick slurry mass on account of the constant agitation of solution and constant temperature. The slurry mass thus formed is left in the reactor and HCL gas is introduced into the reactor. The agitation continues through the process until the slurry mass is filtered out. On getting desired slurry mass by using the aforesaid process, the same is then filtered by passing nitrogen gas through it and keeping the pressure constant between 1.5 to 2 Kgs, while the temperatures ranges between 0°C to 30°C. On filtration, the reactor becomes empty leaving behind a wet cake on agitated filter nutsche. The wet cake is thoroughly washed with Toluene to remove all impurities, while the temperature varies between 15°C to 25°C. Once the wet cake is thoroughly washed and all the possible impurities are removed, then the wet cake is dried to forms an intermediate product known as 3-amino-3- methoxy - N - cyano, 2 - propeneimidate 6 STEP II In order to achieve 3-amino-3 methoxy - N - cyano, 2 - propeneimidate, water is introduced into a Stainless Steel (SS) jacketed reactor having agitator. Thereafter, sodiumbicarbonate and 50% cynamide is introduced, while agitation continues. The temperature of the reactor is reduced and maintained between 0°C to5°C. On reaching the desired temperature, the wet cake prepared in Step I above, is introduced into the reactor. Pursuant to the introduction of the wet cake, agitation is continued for a minimum period of 5 hrs and is allowed to continue until the reaction is completed. On completion of the reaction the temperature of the reactor and mass therein is raised to temperatures ranging between 20°C to 26°C. Once the desired temperature has been reached the same is maintained, while agitation continues for a further period of 2 to 3 hrs. The precipitated slurry mass is then filtered into agitated filter nutsche and the wet cake on the filter is dried. STEP III Once again Toluene is added to the SS reactor and then the dry cake produced in Step II is added to the Toluene solution and heated to reflux. The reactor is heated until the reaching the reflux temperature, which is then maintained until completion of the reaction, while agitation continues throughout the process. The temperature of the reactor is then reduced to temperatures between 55°C to 63°C. On reaching the desired temperature 3% to 8% charcoal is introduced. The reaction mass in the reactor is then filtered into another vessel. On filtration, unwanted contents are left in the 7 reactor, while the Toluene with desired product mass is emptied into another reactor. The reaction mass is thereafter cooled to room temperature and then filtered off to get the desired product of 2-AMINO-4,6-DIMETHOXYPYRIMIDINE in the form of a wet cake which is then dried. The typical example given below to describe the invention do not limit compositional ranges covered under the ambit and scope of the present invention only. Example Stepl In a round bottom flask fitted with mechanical seal stirrer, 1600ml of Toluene is added. The stirring is continued throughout the process. To the Toluene added l00 gms of Methanol is charged at temperatures below 30°C. Subsequent to the mixing of the Toluene and Methanol solution, charged l00gms Malanonitrile is added to said reactor. After charging of Malanonitrile the whole solution is cooled to temperatures 8 ranging between 0°C to 5°C. On reaching the desired cooling temperature, HCL gas is passed through the said solution until the completion of the reaction. At this point, the product formed is Dimethoxy propane Di imino Hydrochloride. After the completion of the reaction, the reaction mass i.e Dimethoxy propane Di imino Hydrochloride is filtered into bunker funnel keeping the temperature below 20°C. On filtration a wet cake of Propane Dimethoxy Di imino Hydrochloride is formed which weighs between 370 gms to 400 gms. The wet cake is further washed with the toluene to remove the impurities present in the wet cake of Dimethoxy Propane Di imino Hydrochloride and the entire mother liquor is recycled and reused after purification to initiate the present chemical reaction. Step 2 In three neck round bottom flask to which is fitted with a mechanical seal stirrer, 800 ml water is charged arid 110 gms of sodium bicarbonate is added to it at room temperature. Then the solution is cooled between 0°C to 2°C. On achieving the desired cooling temperature, the DMM from the step 1 is introduced to the cooled solution. To this cooled solution, 50% cyanamide is added further. Under the continuous stirring, the temperatures is slowly and steadily raised upto 25°C. The reaction mass is stirred for nearly 4 to 7 hrs while the temperature is kept constant. This is done until the reaction is completed. On the completion of the reaction, the mother liquid is filtered under vacuum through buckner filter to leave behind a solid mass of 3-amino-3-methoxy - N - cyano 2-propeimidate while the mother liquid is purified and reused. The wet cake has a weight which may vary between 270 to 300 9 gms. The wet cake will be washed to remove the impurities and then the same is dried to get the moisture content therein below 0.8% to 0.3%. Step 3 Take a three neck round bottom flask fitted with a mechanical seal stirrer to which 700 ml of water is added to which the product Step 2, 3 amino 3 methoxy - N -cyano 2-propeimidate is added at room temperature. Under stirring, 800 ml toluene is further charged. The temperature of the reaction mass is raised to 85 °C to 100°C, while stirring continues. The process of heating continues until the reaction liquid appears to be clear, transparent and homogenous. On the solution becoming clear, transparent and homogenous, 3 to 6 gms of activated carbon is introduced to the solution to remove further impurities which may otherwise remain in the solution. Keeping the temperature constant for a period of 20 to 45 min the solution is stirred. The reaction mass is then filtered through buckenr funnel at the same temperature to remove the carbon in from solution and the impurities that may have removed during the process. The liquid solution on filtration is then transferred into three neck round bottom flask fitted with mechanical seal stirrer. The entire solution is then distilled for removal of toluene, which remains present throughout until the temperature of the solution is constant. On removal of toluene additional 350 to 400 ml water is added under constant stirring. The solution is then cooled upto 30°C to cause crystallization of the finished product. After complete isolation, the wet mass ( 150 to 160 gms ) is filtered through buckner funnel and then the filtrate is purified for reuse, and the 10 crystallized cake is dried to reduce the moisture content to 0.5% to 0.2%. The dried cake is 2-AMINO-4,6-DIMETHOXYPYRIMIDINE, yielding 117 to 125 gms yield. Variations Yield is 1.15 to 1.17 % based on Malanonitrile This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. 11 I CLAIM: 1) A process for preparation of 2-Amino-4,6-Dimethoxypyrimidine comprises: i) charging methanol to mixture of toluene and Malanonitrile at room temperature in NJS jacketed glass line reactor with constant stirring ; ii) passing dry HCL gas passing dry HCL gas to reaction mass of step (i) at temperature varying from 20°C; iii) obtaining. 3-amino-3-methoxy-N - cyano 2-propeimidate after constant stirring and filtration thereof; iv) inoculating the reaction mass of step (iii) to the solution of water, sodium bicarbonate and 50% cynamide maintained at temperatures between 0°C to 5°C; heating, stirring and filtering the reaction mass of step (iv) to produce a slurry; vi) reacting the slurry of step (v) with Toluene to reflux temperature to obtain clear solution; vii) cooling the clear solution of step (vi) between the temperature 55°C to 63°C; 12 viii) adding further the activated char coal to separate unwanted impurities; ix) transferring after filtering the reaction mass of step (viii) into another vessel for cooling to room temperature, thereby obtaining the final product, 2-Amino-4,6-Dimethoxypyrimidine; 2) The method as claimed in claim 1 wherein the ratio Toluene to Malanonitrile varies from 1.15 to 15. 3) The method as claimed in claim 1, wherein the Toluene used is recovered upto 99 to 100% by filtration and distillation. 4) The method as claimed in claim 1, wherein the temperature of 0°to 20°C required for passing HCL gas is maintained by passing chilled water through the cooling jacket. 5) The method as claimed in claim 1, wherein 3-amino-3-methoxy-N-cyano, 2- propeneimidate is reacted with 50% cynamide at temperature between 0°C to 5°C by passing chilled water through jacket; 6) The method as claimed in claim 1, wherein 3-amino-3-methoxy-N- cyano,2propeneimidate is refluxed with Toluene at temperature between 85 to 100°C. 13 7) The method as claimed in claim 1, wherein whole reaction mass is stirred continuously with activated charcoal at temperature between 85 to 100°C until the reaction product appears to be clear, transparent and homogenous. 8) The method as claimed in claim 7, wherein the homogenous product is further washed with water under continuous stirring. 9) The method as claimed in claim 1 wherein the final product, 2-amino-4,6 dimethoxypyrimidine is crystalised out at temperature upto 30°C. 10) The method for producing 2-amino-4,6-dimethoxypyrimidine as herein described substantially and particularly defined in accompanying example. DATED THIS 31st DAY OF JANUARY, 2006. 14 ABSTRACT Accordingly there is provided the process for the preparation of 2- AMINO-4,6-DIMETHOXYPYRIMIDINE which comprises a process for the preparation of 2-Amino-4,6-dimethoxypyrimidine comprises, charging methanol to mixture of Toluene and Malanonitrile at room temperature in MS jacketed glass line reactor With constant stirring ; passing dry HCL gas to reaction mass of step (i in claim 1) at temperature varying from 0°C to 20°C; obtaining 3-amino-3-methoxy-N -2-cyano 2-propeimidate after constant stirring and filtration thereof; inoculating the reaction mass of step (iii in claim 1) to the solution of water, sodium bicarbonate and 50% cynamide maintained at temperatures between 0°C to 5°C;heating, stirring and filtering the reaction mass of step (iv in claim 1) to produce a slurry; reacting the slurry of step (v in claim 1) with Toluene to reflux temperature to obtain clear solution; cooling the clear solution of step (vi in claim 1) between the temperature 55°C to 63CC; adding further the activated char coal to separate unwanted impurities; transferring after filtering the reaction mass of step (viii in claim 1) into another vessel for cooling to room temperature, thereby obtaining the final product, 2-Amino-4,6-Dimethoxypyrimidine;

Documents:

152-mum-2006-abstract(29-11-2007).doc

152-mum-2006-abstract(29-11-2007).pdf

152-mum-2006-abstract.doc

152-mum-2006-abstract.pdf

152-mum-2006-claims(granted)-(29-11-2007).doc

152-mum-2006-claims(granted)-(29-11-2007).pdf

152-mum-2006-claims.doc

152-mum-2006-claims.pdf

152-mum-2006-correspondence 1(18-9-2007).pdf

152-mum-2006-correspondence 2(29-11-2007).pdf

152-mum-2006-correspondence(ipo)-(29-9-2008).pdf

152-mum-2006-correspondence-received.pdf

152-mum-2006-description (complete).pdf

152-mum-2006-drawing(29-11-2007).pdf

152-mum-2006-form 1(31-1-2006).pdf

152-mum-2006-form 18(10-4-2006).pdf

152-mum-2006-form 18(24-9-2007).pdf

152-mum-2006-form 2(granted)-(29-11-2007).doc

152-mum-2006-form 2(granted)-(29-11-2007).pdf

152-mum-2006-form 26(28-12-2005).pdf

152-mum-2006-form 3(31-1-2006).pdf

152-mum-2006-form 9(10-4-2006).pdf

152-mum-2006-form 9(24-9-2007).pdf

152-mum-2006-form-1.pdf

152-mum-2006-form-18.pdf

152-mum-2006-form-2.doc

152-mum-2006-form-2.pdf

152-mum-2006-form-26.pdf

152-mum-2006-form-3.pdf

152-mum-2006-form-9.pdf

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