反应详情

Suspend 3.035 gm. (10 mmole) of methyl 11-chlorodibenzo[b,f][1,4]thiazepin-3-carboxylate in 30 ml. of solfolane (tetrahydrothiophene 1,1-dioxide) and add 766 mg. (20 mmole) of sodium borohydride in small portions with stirring. Stir at room temperature for 3 hours, add a further 190 mg. (5 mmole) of sodium borohydride and continue stirring for 1 hour. Pour the reaction mixture into 100 ml. of ice-water. Extract with three 50 ml. portions of dry ether. Wash the ether extract twice with 50 ml. portions of saturated aqueous sodium chloride, dry over magnesium sulfate and evaporate to a residue. Chromatograph the residue over 100 gm. of silica gel eluting with 1:9 ethyl acetate in toluene. Recrystallize the recovered product from acetonitrile to obtain the title product. (m.p. 149°-150° C.).

1. additionadd a further 190 mg
2. additionPour the reaction mixture into 100 ml
3. extractionExtract with three 50 ml
4. washWash the ether
5. extractionextract twice with 50 ml
6. dry with materialportions of saturated aqueous sodium chloride, dry over magnesium sulfate
7. customevaporate to a residue
8. customRecrystallize the recovered product from acetonitrile