反应详情

Diisobutylaluminium hydride (5.5 ml of a 1M solution in tetrahydrofuran) was added dropwise to 10,11-dihydro-2,8-dimethyl-5H-dibenzo[a,d]cyclohepten-5-one (European Patent, 1993, 0 589 322 A1) (1.2 g) in tetrahydrofuran (20 ml) at-78 ° C. After 1 hour the cooling bath was removed and the reaction was stirred at r.t. for 2 hours. The reaction was quenched with brine and methanol. After 0.5 hours the reaction was partitioned between ethyl acetate and water. The ethyl acetate solution was washed with water, brine, dried (MgSO4) and evaporated. Purification was by chromatography eluting with toluene. Yield 1.2 g. Used directly in step (ii)

1. customAfter 1 hour the cooling bath was removed
2. customThe reaction was quenched with brine and methanol
3. customAfter 0.5 hours the reaction was partitioned between ethyl acetate and water
4. washThe ethyl acetate solution was washed with water, brine
5. dry with materialdried (MgSO4)
6. customevaporated
7. customPurification
8. washeluting with toluene