Acetic Acid → HCID 70069849, compound

Participants

Reaction Steps

1.3 g of dihydrobromide of the B-isomer of ethyl 3-[1(R)-ethoxycarbonyl-2-{2-(4-piperidyl)ethylthio}ethyl]amino-2-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine-1-acetate obtained in Example 5 is dissolved in 10 ml of an aqueous solution of 50% methanol, and the resulting solution is gradually added dropwise to 15.5 ml of an aqueous solution of 2N sodium hydroxide. After stirring for 2 hours at room temperature, the reaction liquid is neutralized with 6.5 ml of acetic acid. The residue obtained by concentration under reduced pressure is purified by HP-20 column chromatography (water:methanol=3:1). The solvent is evaporated under reduced pressure, and the resulting residue is lyophilized to give 440 mg of the B-isomer of 3-[1(R)-carboxy-2-{2-(4-piperidyl)ethylthio}ethyl]amino-2-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine-1-acetic acid monohydrate as a colorless powder.

Provenance & Evidence