反应详情

A mixture of 6.8 g of (+)-cis-2-(4-methoxyphenyl)-3-hydroxy-8-chloro-2,3-dihydro-1,5-benzothiazepin-4(5H)-one, 3.02 g of 2-(dimethylamino)ethyl chloride hydrochloride, 6.1 g of potassium carbonate and 150 ml of acetone is refluxed for 20 hours. After the reaction is completed, insoluble materials are removed by filtration and washed with ethanol. The washings are added to the filtrate, and the combined solution is evaporated under reduced pressure to remove solvent. The residue is dissolved in ethyl acetate, and the solution is washed with water, dried and then evaporated to remove solvent. The residue is recrystallized from a mixture of ethyl acetate and n-hexane. 7.13 g of (+)-cis-2-(4-methoxyphenyl)-3-hydroxy-5-[2-(dimethylamino)ethyl]-8-chloro-2,3-dihydro-1,5-benzothiazepin-4(5H)-one are thereby obtained as colorless needles.

1. temperatureis refluxed for 20 hours
2. custominsoluble materials are removed by filtration
3. washwashed with ethanol
4. additionThe washings are added to the filtrate
5. customthe combined solution is evaporated under reduced pressure
6. customto remove solvent
7. dissolutionThe residue is dissolved in ethyl acetate
8. washthe solution is washed with water
9. customdried
10. customevaporated
11. customto remove solvent
12. customThe residue is recrystallized from a mixture of ethyl acetate and n-hexane