反应详情

A mixture of 2.00 g of 1-amidino-4-piperidinepropionic acid hydrochloride and 0.95 g of p-fluorophenol was suspended in 20 ml of dry pyridine. To the suspension was added with stirring and ice-cooling 1.74 g of dicyclohexylcarbodiimide and the resulting mixture was allowed to stand at room temperature for 4 days. After removal of any insoluble materials, the filtrate was concentrated under reduced pressure. Ethyl acetate was added to the residue to give crystals which were then recrystallized from methanol-ether to obtain 1.4 g (yield: 50.0%) of p-fluorophenyl 1-amidino-4-piperidinepropionate hydrochloride as colorless crystals having a melting point of 131° to 133° C.

1. additionTo the suspension was added
2. customAfter removal of any insoluble materials
3. concentrationthe filtrate was concentrated under reduced pressure
4. additionEthyl acetate was added to the residue
5. customto give crystals which
6. customwere then recrystallized from methanol-ether