HRID1319

反应详情

EQUATION

反应方程式

HRID 1319 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

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).

WORKUP

后处理

  1. filtrationThe mixture was filtered through Celite and filtrate
  2. customwas evaporated to dryness
  3. customThe semi-solid residue was triturated with hexane
  4. customto give 0.63 g