反応 #1415

反応方程式

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

溶媒

ethanol

反応条件

後処理

1. 1
   ろ過The mixture was filtered through Celite and filtrate
2. 2
   その他was evaporated to dryness
3. 3
   その他The semi-solid residue was triturated with hexane
4. 4
   その他to give 0.63 g

実験手順

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).

出典