Abstract: A process of producing 4, 6 Dichloropyrimidine Acid acid, POC13[A2] is charged , 46Dihydroxypyremidine/ N- Methyl-2-Pyrrolidine, which is then heated to 90°C , maintain the temp for 3 hours , add PC13 and chlorine gas (C1↑)[A3] , heat to 110 °C, reflux for 3 to 4 hours , PoC13 is distilled out. The remaining mass/product is distilled out under vacuum at 90°C-110 °C. To eliminate the residue charge chlorinated paraffin.
FORM 2
THE PATENTS ACT, 1970
(39 of 1970)
&
THE PATENT RULES, 2003
COMPLETE SPECIFICATION
Title of Invention:
A process of preparing 4,6-dichloropyrimidine using (NMP) N-Methyl-2-Pyrrolidone.
Name and Address of Applicant:
Sajjan India Limited, #2 Ground Floor, Matulya Centre, Senapati Bapat Marg, Lower Parel, Mumbai-400 013.Maharasthra -INDIA
Following specification particularly describes the nature of invention and the manner, in which it is to be performed.
Field of the Invention
The present invention relates to a process for the preparation of 4,6-dichloropyrimidine (RP-ACID) more particularly, the present invention relates to a process for preparation of 4,6-dichloropyrimidine using N-Methyl-2-Pyrrolidone as a catalyst.
Background /Prior Art
The present invention relates to a process for preparing 4,6-dichloropyrimidine from N-Methyl-2-Pyrrolidone. 4,6-Dichloropyrimidine is a valuable intermediate for preparing crop protection agents.
A number of processes for preparing 4,6-dichloropyrimidine are known, see, for example, W096/23776, EP-A-697 406, EP-A-745 593, WO 95/29166, DE-A-19 53 129 and GB 2 325 224. However, these processes always start from 4,6-dihydroxypyrimidine.
It is also known (see Res. Discl, n 391, 690-691 (1996)) that 4, 6-dichloropyrimidine can be reacted by reacting 4-chloro-6-methoxypyrimidine with a chlorinating agent of the formula R.sub.3 PCl.sub.2.
DE-A44 08 404 describes a process for preparing chloropyrimidines, including inter alia 4,6-dichloropyrimidine. 4,6-dihydroxypyrimidines are generally mentioned as starting material, but not N-Methyl-2-Pyrrolidone. According to this reference, furthermore, chlorination is effected with POCl.sub.3 with addition of amines or amine hydrochlorides.
In the process of manufacturing 4,6-
dichloropyrimidine usually tri ethylene amine is used as a catalyst which at the end of the reaction produces tones of effluent which involves heavy treatment and disposal cost and also invests energy for the same.
No process for preparing 4,6-dichloropyrimidine starting from catalyst N-Methyl-2-Pyrrolidone and resulting in the desired product in a simple manner is yet known.
Objects of the invention
An object of the present invention is that the method employed in this invention saves cost of the effluent treatment and disposal and thereby holds a merit over the known process.
Further important object of the present invention that the process thus described herein saves time and also energy invested for the effluent treatment and hence beneficial in this era of energy crisis.
Further very important object of the present invention is that the use of new reactant in the process resulting in drastic reduction is effluent thereby reducing the cost, manpower, time and economically viable.
SUMMARY OF THE INVENTION
A process of producing 4,6-Dichloropyrimidine, charged POC13[A2] , 4,6-Dihydroxypyrimidine, N-Methyl-2-Pyrrolidone, which is then heated to 90°C and maintain the temp for 3 hours , add PC13 and chlorine gas (Cl2↑)[A3] at 80°C-85°C Then heat to 110 °C, reflux for 3 to 4 hours , PoC13 is distilled out. The remaining mass/product is distilled out under vacuum at 90°C-110 °C. To eliminate the residue charge chlorinated paraffin.[A4]
DETAILED DESRIPTION
A process for preparing 4,6-dichloropyrimidine which is characterized in that N-Metyl-2-Pyrrolidone is reacted with an acid chloride has now been found.
Suitable acid chlorides are selected from the organic and inorganic acid chlorides, for example PCl.sub.3, POCl.sub.3, PCl.sub.5 etc.
The present invention relates to a process for preparing 4, 6-dichloropyrimidine comprising the following process steps , which is characterized in that N-Methyl-2-Pyrrolidone is reacted with an acid chloride has now been found in an alleged invention, in reaction vessel charged PoC13, 4,6-DHP (4,6-dihydroxy pyrimidine), N-Methyl-2-Pyrrolidone, the said reactants have been heated to 25 Degree centigrade to 100°C, and maintained the same temperature for period of 2 to 5 hours, after heating in the reaction mixture the PC13 (Phosphorous Trichloride) is charged and simultaneously chlorine gas (CI2↑) purged in to the reaction mixture, then heated to a temperature between 100 °C to 120°C. The reflux is maintained for 2 to 5 hours, until distillation of PoC13. The resultant reaction mass/product is distilled out under vacuum at 85°C to 120 °C. After
performing the said process if any residue left, to be eliminated charge JB92 (chlorinated paraffin), thereby the required product that is 4,6-dichloropyrimidine is obtained.
DIAGRAM
4,6-Dihydroxy 4,6-Dichloro
Pyrimidine Pyrimidine
RP-Acid
Example:-
In a suitable vessel PoC13 is charged to which 4,6-Dihydroxy Pyrimidine (4,6-DHP) and N-Methyl-2-Pyrrolidone is added. After taking all the reactants, the reaction mixture is heated to 90 °C and the same temperature is maintained for around 3 to 4 hrs. Then charged PC13 and chlorine gas simultaneously at 80°C-85°C. Then heat to 105°C to 110°C and maintain reflux temperature for 2 to 5 hrs. After which POC13 is distilled
out. Then the product is distilled out under vacuum at a vapour temperature of 90-110 °C. In order to eliminate the residue using chlorinated paraffin,
We Claim,
1. A process of preparing 4,6-dichloropyrimidine comprising the following steps, taking in reaction vessel of (NMP) N-Methyl-2-Pyrrolidone in acid chlorides, along with 4, 6 DHP (4, 6 -dihydroxy pyrimidine), the said reactants were heated to 25 Degree centigrade to 100°C, and maintained the same temperature for a period of 2 to 5 hours, after heating the reaction mixture the PC13 (Phosphorous Trichloride) is charged and simultaneously with chlorine gas (Cl2↑) purged in to the reaction mixture followed by heating again at 100 °C to 120°C, the reflux is maintained for 2 to 5 hours, until distillation of PoC13, the resultant reaction mass/product is distilled out under vacuum at 85°C to 120 °C, to obtain a product, followed by elimination of residue,
2. A process as claimed in claim 1, wherein the organic or inorganic acid chlorides are selected from the group consisting of PCl.sub.3, POCl.sub.3, PCl.sub.5 etc.
3. A process as claimed in claim 1, wherein the residue is eliminated using chlorinated paraffin,
4. A process as claimed in claim 1, wherein the reaction temperature maintained 105 °C to 110°C for a period of 3 to 4 hours,
5. A process of preparing 4, 6- dichloropyrimidine such as here in described with reference to an example.
| # | Name | Date |
|---|---|---|
| 1 | 1376-MUM-2010- AFR.pdf | 2022-12-15 |
| 1 | 1376-MUM-2010-FORM 9(21-10-2010).pdf | 2010-10-21 |
| 2 | 1376-MUM-2010-FORM 5(21-10-2010).pdf | 2010-10-21 |
| 2 | 1376-MUM-2010- U. S. PATENT DOCUMENTS.pdf | 2022-12-15 |
| 3 | 1376-MUM-2010-MISCLLENIOUS FORM 30-121021.pdf | 2021-10-18 |
| 3 | 1376-MUM-2010-FORM 18(21-10-2010).pdf | 2010-10-21 |
| 4 | 1376-MUM-2010-CORRESPONDENCE(21-10-2010).pdf | 2010-10-21 |
| 4 | 1376-MUM-2010--CORRESPONDENCE(IPO)-(CERTIFIED COPY LETTER)-(14-10-2021).pdf | 2021-10-14 |
| 5 | 1376-MUM-2010_EXAMREPORT.pdf | 2018-08-10 |
| 6 | 1376-MUM-2010-OTHER DOCUMENT(27-9-2010).pdf | 2018-08-10 |
| 6 | 1376-mum-2010-abstract.pdf | 2018-08-10 |
| 7 | 1376-mum-2010-form 3.pdf | 2018-08-10 |
| 8 | 1376-mum-2010-form 26.pdf | 2018-08-10 |
| 8 | 1376-mum-2010-claims.pdf | 2018-08-10 |
| 9 | 1376-mum-2010-form 2.pdf | 2018-08-10 |
| 9 | 1376-MUM-2010-CORRESPONDENCE(27-9-2010).pdf | 2018-08-10 |
| 10 | 1376-MUM-2010-CORRESPONDENCE(IPO)-(12-2-2014).pdf | 2018-08-10 |
| 11 | 1376-mum-2010-correspondence.pdf | 2018-08-10 |
| 11 | 1376-mum-2010-form 2(title page).pdf | 2018-08-10 |
| 12 | 1376-mum-2010-description(complete).pdf | 2018-08-10 |
| 12 | 1376-mum-2010-form 1.pdf | 2018-08-10 |
| 13 | 1376-mum-2010-description(complete).pdf | 2018-08-10 |
| 13 | 1376-mum-2010-form 1.pdf | 2018-08-10 |
| 14 | 1376-mum-2010-correspondence.pdf | 2018-08-10 |
| 14 | 1376-mum-2010-form 2(title page).pdf | 2018-08-10 |
| 15 | 1376-MUM-2010-CORRESPONDENCE(IPO)-(12-2-2014).pdf | 2018-08-10 |
| 16 | 1376-MUM-2010-CORRESPONDENCE(27-9-2010).pdf | 2018-08-10 |
| 16 | 1376-mum-2010-form 2.pdf | 2018-08-10 |
| 17 | 1376-mum-2010-form 26.pdf | 2018-08-10 |
| 17 | 1376-mum-2010-claims.pdf | 2018-08-10 |
| 18 | 1376-mum-2010-form 3.pdf | 2018-08-10 |
| 19 | 1376-MUM-2010-OTHER DOCUMENT(27-9-2010).pdf | 2018-08-10 |
| 19 | 1376-mum-2010-abstract.pdf | 2018-08-10 |
| 20 | 1376-MUM-2010_EXAMREPORT.pdf | 2018-08-10 |
| 21 | 1376-MUM-2010-CORRESPONDENCE(21-10-2010).pdf | 2010-10-21 |
| 21 | 1376-MUM-2010--CORRESPONDENCE(IPO)-(CERTIFIED COPY LETTER)-(14-10-2021).pdf | 2021-10-14 |
| 22 | 1376-MUM-2010-MISCLLENIOUS FORM 30-121021.pdf | 2021-10-18 |
| 22 | 1376-MUM-2010-FORM 18(21-10-2010).pdf | 2010-10-21 |
| 23 | 1376-MUM-2010-FORM 5(21-10-2010).pdf | 2010-10-21 |
| 23 | 1376-MUM-2010- U. S. PATENT DOCUMENTS.pdf | 2022-12-15 |
| 24 | 1376-MUM-2010-FORM 9(21-10-2010).pdf | 2010-10-21 |
| 24 | 1376-MUM-2010- AFR.pdf | 2022-12-15 |