Refining method for 4,6-dichloro-5-amino-2-propylsulfenyl pyrimidine ester

A technology of propylthiopyrimidinate and refining method, which is applied in the field of refining 4,6-dichloro-5-amino-2-propylthiopyrimidinate, which can solve problems such as difficult removal and final product not meeting quality standards , to achieve the effect of improved appearance, obvious implementation value and high yield

Inactive Publication Date: 2018-03-20
常州沃腾化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the product is not refined, the colored impurities will be carried into the next product, and it is not easy to remove, so that the final product does not meet the quality standard

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Put 50g of reddish-brown 4,6-dichloro-5-amino-2-propylthiopyrimidinate and 450g of cyclohexane into a 1000ml four-neck flask, stir at room temperature under nitrogen protection, then add 100g of washing liquid and stir for 2 hours , the washing solution contains sodium bicarbonate and sodium pyrosulfite, the mass concentration of sodium bicarbonate is 1%, and the mass concentration of sodium pyrosulfite is 1%; standing for stratification, the organic layer is concentrated under reduced pressure at 45 ° C and -0.085 MPa to obtain The residual liquid, the weight ratio of the residual liquid to the organic layer is 1:6, then the residual liquid is cooled to -3°C for crystallization for 3 hours, and filtered to obtain 212g of the mother liquid and the wet product, the wet product is dried under reduced pressure at 8°C and -0.085MPa for 12 hours Obtained 35.5 g of off-white crystalline powder (yield 71%), which is the finished product 4,6-dichloro-5-amino-2-propylthiopyrimidi...

Embodiment 2

[0016] In a 2000ml four-necked flask, drop into reddish-brown 4,6-dichloro-5-amino-2-propylthiopyrimidinate 50g, mother liquor weight 212g and fresh cyclohexane 390g in example 1, stir under nitrogen protection at room temperature , then add washing solution 200g and stir for 4 hours, containing sodium bicarbonate and sodium pyrosulfite in the washing solution, the mass concentration of sodium bicarbonate is 1%, and the mass concentration of sodium pyrosulfite is 1%; ℃, -0.085MPa and concentrated under reduced pressure to obtain the residual liquid, the weight ratio of the residual liquid to the organic layer is 1:6, then the residual liquid is cooled to -3°C for crystallization for 3 hours, and filtered to obtain 223g of the mother liquor and wet product, the wet product is 8°C , -0.085MPa and dried under reduced pressure for 12 hours to obtain 47g of off-white crystalline powder (93.1% yield), which is the finished product 4,6-dichloro-5-amino-2-propylthiopyrimidinate.

Embodiment 3

[0018] Put 50g of reddish-brown 4,6-dichloro-5-amino-2-propylthiopyrimidine ester and 456g of petroleum ether (30-60℃) into a 1000ml four-neck flask, stir at room temperature under nitrogen protection, and then add 100g of the washing solution was stirred for 2 hours, and the washing solution contained sodium bicarbonate and sodium pyrosulfite, the mass concentration of sodium bicarbonate was 1%, and the mass concentration of sodium pyrosulfite was 1%; standing for stratification, the organic layer was heated at 45 ° C, - Concentrate under reduced pressure at 0.085MPa to obtain the residual liquid, the weight ratio of the residual liquid to the organic layer is 1:6, then cool the residual liquid to -3°C for crystallization for 3 hours, filter to obtain 187g of mother liquor and wet product, wet product at 8°C, - Dry under reduced pressure at 0.085MPa for 12 hours to obtain 37.1 g (yield 74.2%) of off-white crystalline powder, which is the finished product 4,6-dichloro-5-amino-2...

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PUM

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Abstract

The invention relates to a refining method for 4,6-dichloro-5-amino-2-propylsulfenyl pyrimidine ester. The refining method is characterized by comprising the following steps: adding a reddish brown 4,6-dichloro-5-amino-2-propylsulfenyl pyrimidine ester crude product and a solvent into a reactor, stirring at room temperature under protection of nitrogen gas, adding a washing solution, standing andlayering after stirring, taking an organic layer to concentrate under reduced pressure to obtain residual fluid; cooling, crystallizing and filtering the residual fluid to obtain a wet product; and drying the wet product under reduced pressure to obtain off-white crystalline powder, thereby obtaining refined 4,6-dichloro-5-amino-2-propylsulfenyl pyrimidine ester. The refining method has the advantages of being environmentally friendly, simple in process and high in economical efficiency.

Description

technical field [0001] The invention relates to a method for refining an antiplatelet drug intermediate, in particular to a method for refining 4,6-dichloro-5-amino-2-propylthiopyrimidinate. Background technique [0002] 4,6-dichloro-5-amino-2-propylthiopyrimidinate is an important intermediate of ticagrelor, a highly effective antiplatelet drug developed by AstraZeneca. The synthesis process patent of this compound is WO2000034283A1. Oxidation impurities are easily produced due to the presence of amino groups during the synthesis process and storage process, making the appearance of the product orange-red to brown-black. If the product is not refined, the colored impurities will be brought into the next product, and it is more difficult to remove, so that the final product does not meet the quality standards. Therefore, an environment-friendly, simple process and high economical refining process has high practicability. Contents of the invention [0003] In view of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/47
CPCC07D239/47
Inventor 孙富强万志兵李大娟
Owner 常州沃腾化工科技有限公司
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