反应详情

Triethylamine (0.42 mL, 3.0 mmol) was added to a mixture of 4-[(tert-butoxycarbonyl)amino]cyclohexanecarboxylic acid (1.0 mmol), dimethylamine (0.6 mL, 1.2 mmol) (2 N THF solution) and benzotriazol-1-yloxytris(dimethylamino)phosphonium hexafluorophosphate (0.46 g, 1.1 mmol) in methylene chloride (5.0 mL). The mixture was stirred at r.t. overnight. The mixture was diluted with water, and extracted with ethyl acetate (3×10 mL). The combined organic layers were dried over MgSO4, filtered and concentrated. The residue was purified by flash chromatography on a silica gel column with ethyl acetate in hexanes (0-40%) to afford the desired product (0.20 g, 74%). Analytic LCMS (M+Na)+: m/z=293.1; (M-Boc+H)+: m/z=171.1.

1. extractionextracted with ethyl acetate (3×10 mL)
2. dry with materialThe combined organic layers were dried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue was purified by flash chromatography on a silica gel column with ethyl acetate in hexanes (0-40%)