反应详情

A mixture of 8.2 g of (±)-cis-2-(4-methoxyphenyl)-3-hydroxy-7,8-dimethyl-2,3-dihydro-1,5-benzothiazepin-4(5H)-one, 3.1 g of potassium hydroxide and 100 ml of dimethylsulfoxide is stirred at room temperature for 30 minutes. Then, 4 g of 2-(dimethylamino)ethyl chloride hydrochloride are added to the mixture, and said mixture is stirred at room temperature for 20 hours. After the reaction is completed, the mixture is poured into ice-water. The aqueous mixture is extracted with ethyl acetate, and the ethyl acetate layer is further extracted with 20% hydrochloric acid. The hydrochloric acid layer is alkalized with conc. aqueous ammonia, and the precipitated crystals are collected by filtration, washed with water and then dried. 6.4 g of (±)-cis-2-(4-methoxyphenyl)-3-hydroxy-5-[2-(dimethylamino)ethyl]-7,8-dimethyl-2,3-dihydro-1,5-benzothiazepin-4(5H)-one are obtained.

1. stirringis stirred at room temperature for 20 hours
2. extractionThe aqueous mixture is extracted with ethyl acetate
3. extractionthe ethyl acetate layer is further extracted with 20% hydrochloric acid
4. filtrationthe precipitated crystals are collected by filtration
5. washwashed with water
6. customdried