A kind of synthetic method of atorvastatin calcium intermediate
A technique for synthesizing atorvastatin calcium, which is applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., and can solve the problem of large volume ratio difference between catalyst and raw material and continuous operation Insufficient compatibility, poor mixing effect and other problems, to achieve the effect of low production cost, short reaction time and high degree of automation
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0023] Under nitrogen protection, add 1000g of compound II and 700g of 2,2-dimethoxypropane into a 2L three-necked flask, start stirring, and cool down to about 10°C after compound II is dissolved. 75 g of Amberlite-15 acidic resin was filled in fixed bed reactor 1, and 75 g of Amberlite IRA-93 basic resin was filled in fixed bed reactor 2 . Use a metering pump to pump the mixture of compound II and 2,2-dimethoxypropane into the fixed-bed reactor 1 filled with acidic resin for catalytic reaction, the reaction temperature is 15°C, and the time is 40s. After the reaction is completed, the The obtained reaction liquid was pumped into the fixed-bed reactor 2 filled with basic resin for quenching, the quenching temperature was 15°C, and the quenching time was 40s. During the reaction, take a sample of the TLC control (take the reaction solution, add a small amount of triethylamine to adjust the pH to alkaline, spot the plate, KMnO 4 Color development), when compound II disappears ...
Embodiment 2
[0025] Under the protection of nitrogen, add 1000g of compound II and 900g of 2,2-dimethoxypropane into a 2L three-necked flask, start stirring, and cool down to about 10°C after compound II is dissolved. Fixed-bed reactor 1 was filled with 40 g of Amberlite-15 acidic resin, and fixed-bed reactor 2 was filled with 40 g of Amberlite IRA-93 basic resin. Use a metering pump to pump the mixture of compound II and 2,2-dimethoxypropane into the fixed-bed reactor 1 filled with acidic resin for catalytic reaction, the reaction temperature is 25°C, and the time is 20s. After the reaction is completed, the The obtained reaction liquid was pumped into the fixed-bed reactor 2 filled with basic resin for quenching, the quenching temperature was 25°C, and the quenching time was 20s. During the reaction, take a sample of the TLC control (take the reaction solution, add a small amount of triethylamine to adjust the pH to alkaline, spot the plate, KMnO 4 Color development), when compound II d...
Embodiment 3
[0027]Under the protection of nitrogen, add 1000g of compound II and 500g of 2,2-dimethoxypropane into a 2L three-necked flask, start stirring, and cool down to about 10°C after compound II is dissolved. Fixed-bed reactor 1 was filled with 90 g of Amberlite-15 acidic resin, and fixed-bed reactor 2 was filled with 90 g of Amberlite IRA-93 basic resin. Use a metering pump to pump the mixed solution of compound II and 2,2-dimethoxypropane into the fixed bed reactor 1 filled with acidic resin to carry out the catalytic reaction, the reaction temperature is 5°C, and the time is 60s. After the reaction is completed, the The obtained reaction solution was pumped into the fixed-bed reactor 2 filled with basic resin for quenching, the quenching temperature was 5°C, and the quenching time was 60s. During the reaction, take a sample of the TLC control (take the reaction solution, add a small amount of triethylamine to adjust the pH to alkaline, spot the plate, KMnO 4 Color development),...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More