반응 #73717
ord-6d9c85febd71411d978afb7779d446c3
반응 방정식
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도under reflux for 6 hr
- 2여과The reaction mixture was filtered through Celite
- 3세척the filter cake was washed with ethyl acetate
- 4기타The solvent was removed on a rotary evaporator
- 5기타the crude product was purified by chromatography on silica (110 g) with 5% ethyl acetate in heptane (5 L)
- 6기타to produce 4 (2.75 g, 64% over 2 steps)
실험 절차
A solution of crude 3 (10.25 mmol) in dichloromethane (160 mL) was treated with manganese dioxide (14 g, 15 equiv.) and this suspension was stirred under reflux for 6 hr. The reaction mixture was filtered through Celite and the filter cake was washed with ethyl acetate. The solvent was removed on a rotary evaporator and the crude product was purified by chromatography on silica (110 g) with 5% ethyl acetate in heptane (5 L) to produce 4 (2.75 g, 64% over 2 steps).