Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of refining method of rosuvastatin calcium intermediate

A technology of rosuvastatin calcium and a refining method, which is applied in the field of preparation of pharmaceutical compounds, can solve the problems that there is no method to improve the purity, and achieve the effect of facilitating distillation and separation and improving the purity

Active Publication Date: 2019-05-07
ABA CHEM SHANGHAI
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the literature reports on the research on the quality standard of 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methylsulfonyl)amino]pyrimidine-5-methanol only have its residual Solvent determination and content determination, but there is no improvement in rosuvastatin calcium intermediate 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methylsulfonyl)amino] Method for the purity of pyrimidine-5-methanol

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of refining method of rosuvastatin calcium intermediate
  • A kind of refining method of rosuvastatin calcium intermediate
  • A kind of refining method of rosuvastatin calcium intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Purification of rosuvastatin calcium intermediate 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methylsulfonyl)amino]pyrimidine-5-methanol in this example Method, the refining method concrete steps are as follows:

[0024] (1) 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methylsulfonyl)amino]pyrimidine-5 with a molar mass of 12 mol and a purity of 98% - Put the crude methanol into the reactor, then add 12 mol of ethanol into the reactor, and stir for 6 minutes by a stirrer with a rotation speed of 60r / min to make 4-(4-fluorophenyl)-6-isopropyl-2-[ (N-methyl-N-methylsulfonyl)amino]pyrimidine-5-methanol crude product is all dissolved in an organic solvent;

[0025] (2) Send the crude product of 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methylsulfonyl)amino]pyrimidine-5-methanol miscible in ethanol to To the distillation tower, the temperature was raised to 70°C within 1 hour, and kept for distillation for 20 minutes; then the temperature was raised to 80°C within 3...

Embodiment 2

[0028] Purification of rosuvastatin calcium intermediate 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methylsulfonyl)amino]pyrimidine-5-methanol in this example Method, the refining method concrete steps are as follows:

[0029] (1) 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methylsulfonyl)amino]pyrimidine-5 with a molar mass of 12 mol and a purity of 98.5% -Put the crude methanol into the reactor, then add 24mol of ethanol into the reactor, and stir for 4min with a stirrer with a rotation speed of 70r / min to make 4-(4-fluorophenyl)-6-isopropyl-2-[ (N-methyl-N-methylsulfonyl)amino]pyrimidine-5-methanol crude product is all dissolved in an organic solvent;

[0030] (2) Send the crude product of 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methylsulfonyl)amino]pyrimidine-5-methanol miscible in ethanol to To the distillation tower, the temperature was raised to 70°C within 1 hour, and kept for distillation for 20 minutes; then the temperature was raised to 80°C within 30 m...

Embodiment 3

[0033] Purification of rosuvastatin calcium intermediate 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methylsulfonyl)amino]pyrimidine-5-methanol in this example Method, the refining method concrete steps are as follows:

[0034] (1) 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methylsulfonyl)amino]pyrimidine-5 with a molar mass of 12 mol and a purity of 98.25% -Put the crude methanol into the reactor, then add 18 mol of ethanol into the reactor, and stir for 5 minutes by a stirrer with a rotation speed of 65r / min to make 4-(4-fluorophenyl)-6-isopropyl-2-[ (N-methyl-N-methylsulfonyl)amino]pyrimidine-5-methanol crude product is all dissolved in an organic solvent;

[0035] (2) Send the crude product of 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methylsulfonyl)amino]pyrimidine-5-methanol miscible in ethanol to To the distillation tower, the temperature was raised to 70°C within 1 hour, and kept for distillation for 20 minutes; then the temperature was raised to 80°C within...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a refining method of a rosuvastatin calcium intermediate, namely 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methylsulfonyl)amino]pyrimidine-5- methanol. The refining method specifically includes completely dissolving a crude product of the 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methylsulfonyl)amino]pyrimidine-5- methanol with the purity of 98-98.5% in organic solvent; feeding the organic solvent to a distillation tower for distillation to obtain a semi-finished product of the 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methylsulfonyl)amino]pyrimidine-5-methanol; feeding the semi-finished product to a condensation tower for concentration to obtain the 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methylsulfonyl)amino]pyrimidine-5-methanol. The refining method has the advantages that through mixed dissolving and distillation, the purity of the 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methylsulfonyl)amino]pyrimidine-5-methanol is improved greatly and can reach more than 99.8%.

Description

technical field [0001] The invention belongs to the technical field of preparation of pharmaceutical compounds, in particular to a rosuvastatin calcium intermediate 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methylsulfonyl ) Amino] [0002] Purification method of pyrimidine-5-methanol. Background technique [0003] Rosuvastatin calcium (Rosuvastatin calcium) is a new type of 3-hydroxy-3-methylglutaryl coenzyme A (HMG CoA) reductase inhibitor. It is the seventh statin drug to enter the market and is the strongest so far. Effective lipid-lowering drugs, known as "super statins", are mainly used to treat hyperlipidemia and hypercholesterolemia. [0004] 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methylsulfonyl)amino]pyrimidine [0005] -5-Methanol is an intermediate in the synthesis of rosuvastatin calcium. Drug synthesis intermediates are important substances in the synthesis of raw materials, and their quality directly determines the quality and curative effect of r...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/42
CPCC07D239/42
Inventor 蒋信义徐萌周宇肖方亮
Owner ABA CHEM SHANGHAI