反应详情

A mixture of (+)-cis-2-(4-methoxyphenyl)-3-hydroxy-8-chloro-2,3-dihydro-1,5-benzothiazepin-4(5H)-one (6.8 g), 2-(dimethylamino)ethyl chloride hydrochloride (3.02 g), potassium carbonate (6.1 g) and acetone (150 ml) is stirred under refluxing for 20 hours. After the completion of the reaction, the insoluble materials are removed by filtration and the filtrate is concentrated under reduced pressure. The resulting residue is dissolved in ethyl acetate, washed with water, dried and the ethyl acetate is distilled off. The resulting residue is recrystallized from a mixture of ethyl acetate and n-hexane to give (+)-cis-2-(4-methoxyphenyl)-3-hydroxy-5-[2-(dimethylamino)ethyl]-8-chloro-2,3-dihydro-1,5-benzothiazepin-4(5H)-one (7.13 g) as colorless needles, m.p. 122°-124° C. (decomposed).

1. temperatureunder refluxing for 20 hours
2. customAfter the completion of the reaction
3. customthe insoluble materials are removed by filtration
4. concentrationthe filtrate is concentrated under reduced pressure
5. dissolutionThe resulting residue is dissolved in ethyl acetate
6. washwashed with water
7. customdried
8. distillationthe ethyl acetate is distilled off
9. customThe resulting residue is recrystallized from a mixture of ethyl acetate and n-hexane