反应详情

A mixture of 0.25 g of diphenylmethyl α-[4-[4-(4-benzyloxycarbonylamidinophenoxy)butyl]-2,3-dioxopiperazin-1-yl]-α-phenylacetate, 0.13 g of 5% palladium-carbon, 0.34 ml of 1N hydrochloric acid and 5 ml of N,N-dimethylformamide was subjected to hydrogenation at ordinary temperature and atmospheric pressure for 3 hours. Then, the pallasium-carbon was filtered off and the filtrate was concentrated under reduced pressure. To the resulting residue were added 2 ml of ethyl acetate, 5 ml of water and 30 mg of sodium hydrogencarbonate to dissolve the residue. The aqueous layer was separated and then purified by a reversed phase column chromatography (eluent: a 50% aqueous acetonitrile solution) to obtain 0.10 g of α-[4-[4-(4-amidinophenoxy)butyl]-2,3-dioxopiperazin-1-yl]-α-phenylacetic acid as colorless crystals.

1. filtrationThen, the pallasium-carbon was filtered off
2. concentrationthe filtrate was concentrated under reduced pressure
3. additionTo the resulting residue were added 2 ml of ethyl acetate, 5 ml of water and 30 mg of sodium hydrogencarbonate
4. dissolutionto dissolve the residue
5. customThe aqueous layer was separated
6. custompurified by a reversed phase column chromatography (eluent