反应详情

A mixture of 985 mg of (-)-cis-2-(4-methoxyphenyl)-3-propionyloxy-5-[2-(N-benzyloxycarbonyl-N-methylamino)ethyl]-8-chloro-2,3-dihydro-1,5-benzothiazepin-4(5H)-one, 1.6 ml of 25% hydrogen bromide-acetic acid and 5 ml of benzene is stirred for 5 hours under ice-cooling. Then, the mixture is evaporated at room temperature to remove benzene. Ether is added to the residue, and the precipitates are collected by filtration and washed with ether. Water is added to said precipitates, and the aqueous mixture is neutralized with potassium carbonate and extracted with ethyl acetate. The extract is washed with water, dried and evaporated under reduced pressure to remove solvent. 660 mg of (-)-cis-2-(4-methoxyphenyl)-3-propionyloxy-5-[2-(N-methylamino)ethyl]-8-chloro-2,3-dihydro-1,5-benzothiazepin-4(5H)-one are obtained as caramel.

1. temperaturecooling
2. customThen, the mixture is evaporated at room temperature
3. customto remove benzene
4. additionEther is added to the residue
5. filtrationthe precipitates are collected by filtration
6. washwashed with ether
7. additionWater is added
8. customto said precipitates
9. extractionextracted with ethyl acetate
10. washThe extract is washed with water
11. customdried
12. customevaporated under reduced pressure
13. customto remove solvent