反应详情

A solution of (2R)-1-[3,5-bis(trifluoromethyl)benzoyl]-4-[[1-(tert-butoxycarbonylmethyl)-1H-pyrazol-4-yl]methyl]-2-(3,4-dimethylbenzyl)piperazine (425 mg) in dichloromethane (2.5 ml) was treated with trifluoroacetic acid (2.5 ml) at room temperature for 1 hour. The mixture was adjusted to pH 7.4 with aqueous sodium bicarbonate solution and evaporated under reduced pressure. The residue was washed with a mixture of dichloromethane and methanol (9:1), and the solution was evaporated under reduced pressure and purified by column chromatography on a silica gel using a mixture of methanol and chloroform (1:9) as eluent and subsequent crystallization from ethyl acetate, isopropyl ether, and hexane to give (2R)-1-[3,5-bis(trifluoromethyl)benzoyl]-4-[[1-(carboxymethyl)-1H-pyrazol-4-yl]methyl]-2-(3,4-dimethylbenzyl)piperazine (395 mg) as a white powder.

1. customevaporated under reduced pressure
2. washThe residue was washed with a mixture of dichloromethane and methanol (9:1)
3. customthe solution was evaporated under reduced pressure
4. custompurified by column chromatography on a silica gel using
5. additiona mixture of methanol and chloroform (1:9) as eluent
6. customsubsequent crystallization from ethyl acetate, isopropyl ether, and hexane