反应详情

温度

110 °C

A mixture of 1 g of (±)-cis-2-(4-methoxyphenyl)-3-hydroxy-5-[2-(dimethylamino)ethyl]-8-chloro-2,3-dihydro-1,5-benzothiazepin-4(5H)-one hydrochloride, 2 ml of acetic anhydride and 2 ml of acetic acid is stirred at 110° C. for 4 hours. Then, the reaction mixture is evaporated under reduced pressure to remove solvent. Ether is added to the residue, and the precipitated crystals are collected by filtration. 1.08 g of (±)-cis-2-(4-methoxyphenyl)-3-acetoxy-5-[2-(dimethylamino)ethyl]-8-chloro-2,3-dihydro-1,5-benzothiazepin-4(5H)-one hydrochloride are thereby obtained. Recrystallization of the product from a mixture of chloroform, ethanol and ether gives crystals (needles) melting at 159°-161° C.

1. customThen, the reaction mixture is evaporated under reduced pressure
2. customto remove solvent
3. additionEther is added to the residue
4. filtrationthe precipitated crystals are collected by filtration