反应详情

To a mixture of 6-Methoxy-1-indanone (15 g, 92.6 mmol), sodium azide (26.7 g, 277.8 mmol), in CHCl3 was added methane sulfonic acid (60 g, 926 mmol) via addition funnel at 0° C. Reaction mixture was warm to room temperature. Stirring was continued for 3 hr, then poured into cold water. The organics were extracted with methylene chloride and washed with water, sat. NaCl and dried over Na2SO4. Organic solution was concentrated in vacuo and the residue was purified with silica gel eluting with 20% EtOAc/Hexane to give the title compound as a yellow solid (10.5 g, 63%). MS (ES) m/z 178.1.

1. additionvia addition funnel at 0° C
2. customReaction mixture
3. extractionThe organics were extracted with methylene chloride
4. washwashed with water, sat. NaCl
5. dry with materialdried over Na2SO4
6. concentrationOrganic solution was concentrated in vacuo
7. customthe residue was purified with silica gel eluting with 20% EtOAc/Hexane