Hydrogen chloride-ethyl acetate → HCID 70044618, compound

Participants

Reaction Steps

In 100 ml of hydrogen chloride-ethyl acetate (5N) solution is dissolved 0.4 g of tert-butyl 3(S)-[1(S)-ethoxycarbonyl-3-phenylpropyl]amino-4-oxo-2,3,4,5-tetrahydro-1,5-benzoxazepine-5-yl-N-acetyl-L-phenylalaninate obtained in Example 24 and the solution is allowed to stand for 4 hours. The reaction solution is concentrated under reduced pressure, and 50 ml of ether is added to the residue. The resulting mixture is extracted twice with 70 ml each of saturated sodium bicarbonate solution and the aqueous layer is extracted with 50 ml of ether. The aqueous layer is neutralized with 1N hydrochloric acid and extracted with 100 ml of ethyl acetate. The ethyl acetate layer is dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The oily product is dissolved in 10 ml of ether, and 0.5 ml of hydrogen chloride-ethyl acetate (5N) solution is added to the solution to give 0.2 g of 3(S)-[1(S)-ethoxycarbonyl-3-phenylpropyl]amino-4-oxo-2,3,4,5-tetrahydro-1,5-benzoxazepine-5-yl-N-acetyl-L-phenylalanine hydrochloride as a colorless powder.

Provenance & Evidence