反应详情

To a stirred mixture of trans-4-tert-butoxycarbonylamino-cyclohexanecarboxylic acid (6.1 g, 25.0 mmol) and cyclopropylamine (1.9 mL, 27.5 mmol) in dichloromethane (125 mL), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (5.3 g; 27.5 mmol) is added in one portion. The reaction is stirred at ambient temperature for 48 hours. The solvent is evaporated and the crude is stirred in ice-cold 1N hydrochloric acid (100 mL) for 30 min. The solid product is isolated by suction filtration, washed with small portions of water and recrystallized from ethanol/water to deliver 5.2 g of the title compound as colorless solid.

1. additionis added in one portion
2. customThe solvent is evaporated
3. stirringthe crude is stirred in ice-cold 1N hydrochloric acid (100 mL) for 30 min
4. customThe solid product is isolated by suction filtration
5. washwashed with small portions of water
6. customrecrystallized from ethanol/water