反应详情

To a mixture of 13 g of 2,3-dihydrothieno[3,2-f][1,4]thiazepin-5(4H)-one and 21.5 g of 4-chlorobutyryl chloride in 200 ml of dichloroethane was added 21.5 g of aluminum chloride under cooling and the mixture was stirred for 3 hours. The mixture was poured into ice-cold water and extracted with chloroform. The organic layer was washed with saline solution, dried over magnesium sulfate and concentrated. The residue was recrystallized from ethanol to give 12 g of 7-(4-chlorobutyryl)-2,3-dihydrothieno[3,2-f][1,4]thiazepin-5(4H)-one as white crystals, m.p. 124°-125° C.

1. temperatureunder cooling
2. additionThe mixture was poured into ice-cold water
3. extractionextracted with chloroform
4. washThe organic layer was washed with saline solution
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated
7. customThe residue was recrystallized from ethanol