反应详情

Cool a solution of 17 g 2-methylcycloheptanone in 75 ml concentrated hydrochloric acid and add protionwise 13.2 g sodium azide. Stir the reaction of 0° for 1 hour then at room temperature for 2 hours. Add the reaction to 150 ml ice water, bring to pH 7 with potassium carbonate and extract with chloroform. Treat the extracts with charcoal, dry over MgSO4, filter and concentrate to obtain crude 8-methylperhydroazocin-2-one. Obtain a pure product by recrystallization from hexane (m.p. 70-73).

1. customthe reaction of 0° for 1 hour
2. additionAdd
3. extractionextract with chloroform
4. additionTreat the extracts with charcoal
5. dry with materialdry over MgSO4
6. filtrationfilter
7. concentrationconcentrate