반응 #1415
ord-d232c1adede245b1b40453d6829ded7a
반응 방정식
chloroform
methanol
(S)-1,3,4,5-tetrahydro-4-[[(phenylmethoxy)carbonyl]amino]-3-oxo-2H-2-benzazepine-2-acetic acid, ethyl ester
methylene chloride
→
(S)-1,3,4,5-Tetrahydro-4-amino-3-oxo-2H-2-benzazepine-2-acetic acid, ethyl ester
반응물
용매
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1여과The mixture was filtered through Celite and filtrate
- 2기타was evaporated to dryness
- 3기타The semi-solid residue was triturated with hexane
- 4기타to give 0.63 g
실험 절차
20% Palladium hydroxide/carbon catalyst was added to a solution of (S)-1,3,4,5-tetrahydro-4-[[(phenylmethoxy)carbonyl]amino]-3-oxo-2H-2-benzazepine-2-acetic acid, ethyl ester (1.037 g., 2.62 mmole) in absolute ethanol (20 ml.) and the resulting suspension was stirred under a hydrogen atmosphere (balloon) for 2 hours. The mixture was filtered through Celite and filtrate was evaporated to dryness. The semi-solid residue was triturated with hexane to give 0.63 g. of product as a white, crystalline solid; m.p. 71°-73° C.; Rf =0.38 (methanol:methylene chloride, 1:9); [α]D =77.5° (c=0.59, chloroform).