反应详情

Suspend 6.7 gm. (20 mmole) of methyl 11-chlorodibenzo[b,f][1,4]thiazepin-3-carboxylate 5,5-dioxide in 60 ml. of sulfolane and stir under nitrogen at room temperature while adding 1.52 g. (40 mmole) of sodium borohydride in small portions. Control foaming, if desired, by adding small portions of dry ether. After 2 hours, pour the reaction mixture into 300 ml. of ice-water and 75 ml. of ether. Separate the precipitate by filtration, wash with water and dry in vacuo. Dissolve the precipitate in 175 ml. of boiling acetonitrile, filter and concentrate to 100 ml. Separate the precipitate to obtain the title product. (m.p. 236° C.)

1. additionwhile adding 1.52 g
2. additionpour the reaction mixture into 300 ml
3. customSeparate the precipitate
4. filtrationby filtration
5. washwash with water
6. customdry in vacuo
7. dissolutionDissolve the precipitate in 175 ml
8. filtrationof boiling acetonitrile, filter
9. concentrationconcentrate to 100 ml
10. customSeparate the precipitate