反应详情

Trifluoroacetic acid (1.5 ml) was added to a solution of crude [4-hydroxy-4-(1-phenyl-ethylcarbamoyl)-cyclohexyl]-carbamic acid tert-butyl ester (320 mg) in dichloromethane (6.0 ml). The reaction was judged to be complete by LCMS in less than 90 minutes. The reaction was diluted with dichloromethane and quenched to pH 12 using 5N sodium hydroxide. The crude product was extracted with two volumes of dichloromethane, dried over sodium sulfate, filtered and concentrated to 4-amino-1-hydroxy-cyclohexanecarboxylic acid (1-phenyl-ethyl)-amide (210 mg). LCMS M+H=263.2.

1. waitto be complete by LCMS in less than 90 minutes
2. customquenched to pH 12
3. extractionThe crude product was extracted with two volumes of dichloromethane
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated to 4-amino-1-hydroxy-cyclohexanecarboxylic acid (1-phenyl-ethyl)-amide (210 mg)