Method for synthesizing Lomerizine Hydrochlortde
A technology of lomerizine hydrochloride and its synthesis method, which is applied in the direction of organic chemistry, etc., and can solve the problems of low industrial production value, low yield of lomerizine hydrochloride synthesis technology, and difficulty in obtaining medicinal crystal forms of lomerizine hydrochloride To achieve the effect of shortening treatment time, reasonable treatment, and relieving pain
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[0020] Example 1:
[0021] Put 1020g of 2,3,4-trimethoxybenzaldehyde and 1500g of bis(4-fluorophenyl)methylpiperazine into the reaction flask and slowly melt it in an oil bath at 100°C. After melting is complete, slowly add 260ml of formic acid dropwise. After dripping, continue to stir and react at this temperature for 1 hour, cool to room temperature, add 960ml of concentrated hydrochloric acid (37%) and 9600ml of absolute ethanol and stir and reflux for 1 hour, then add 60g of activated carbon, and continue to stir and decolorize for 0.5 hours. After filtering, the filtrate is slowly cooled and crystallized to obtain 2507.4 g of white crystals, with a yield of 90.02%, mp: 202°C (document mp: 204°C) mother liquor is recovered and cooled to obtain crude Lomerizine hydrochloride, which can increase the yield.
[0022] Take 1950.3g of crude Lomerizine Hydrochloride and add 7000ml of acetonitrile-methanol (80%-20%) mixed solution, stir and heat for 1 hour, cool and filter to obtain ...
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[0023] Example 2:
[0024] Put 1020g of 2,3,4-trimethoxybenzaldehyde and 3750g of bis(4-fluorophenyl)methylpiperazine into the reaction flask and slowly melt it in an oil bath at 100°C. After melting is complete, slowly add 260ml of formic acid dropwise. After dripping, continue to stir and react at this temperature for 3 hours, cool to room temperature, add 960ml of concentrated hydrochloric acid (37%) and 9600ml of absolute ethanol and stir and reflux for 5 hours, then add 90g of activated carbon, and continue to stir and decolorize for 1 hour. After filtering, the filtrate was slowly cooled and crystallized to obtain 2548.6 g of white crystals with a yield of 91.5%, mp: 202°C (document mp: 204°C).
[0025] Take 1950.3 g of crude Lomerizine hydrochloride and add 7000 ml of acetonitrile-ethanol (80%-20%) mixed solution, heat for 1 hour with stirring, cool and filter to obtain white crystals, and dry to obtain 1057.7 g of refined products. The yield is 54.23%, mp: 207.8-208.9°C.
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