反应详情

To a cold solution (-4° C.) of (1-methylcyclohexyl)methanol (6.2 g, 0.048 mol) in DMF (90 ml) was added 50% oily sodium hydride (2.81 g, 0.059 mol as NaH). After stirring for 1 hr, sulfamoyl chloride (7.82 g, 0.062 mol) was added and the stirring was continued for an additional 30 min at -4° C. The reaction mixture was poured into cold water and extracted with toluene. The organic layer was dried (Na2SO4) and the solvents were removed under vacuum to give a syrup which crystallized upon cooling. Recrystallization from chloroform/hexane gave pure (1-methylcyclohexyl)methane sulfamate, mp 40°-42° C.

1. waitthe stirring was continued for an additional 30 min at -4° C
2. extractionextracted with toluene
3. dry with materialThe organic layer was dried (Na2SO4)
4. customthe solvents were removed under vacuum
5. customto give a syrup which
6. customcrystallized
7. temperatureupon cooling
8. customRecrystallization from chloroform/hexane