反应详情

Under nitrogen atmosphere, to a mixture of (2R)-1-[3,5-bis(trifluoromethyl)benzoyl]-2-(3,4-dimethylbenzyl)piperazine (315 mg) and 3-(1-methyl-1H-imidazol-4-yl)propanal (98 mg) in dichloromethane (6 ml) was added sodium triacetoxyborohydride (225 mg) and'stirred at room temperature. After 4 hours, aqueous sodium bicarbonate solution was added to the mixture and the mixture was stirred for several minutes. The organic layer was separated, dried over sodium sulfate and evaporated under reduced pressure. The resulting residue was purified by column chromatography on silica gel using dichloromethanemethanol (10:1) as eluent and treated with 4N hydrogen chloride in ethyl acetate solution to give (2R)-1-[3,5-bis(trifluoromethyl)benzoyl]-2-(3,4-dimethylbenzyl)-4-[3-(1-methyl-1H-imidazol-4-yl)propyl]piperazine dihydrochloride (187.1 mg).

1. customat room temperature
2. customThe organic layer was separated
3. dry with materialdried over sodium sulfate
4. customevaporated under reduced pressure
5. customThe resulting residue was purified by column chromatography on silica gel using dichloromethanemethanol (10:1) as eluent
6. additiontreated with 4N hydrogen chloride in ethyl acetate solution