HRID743429

反应详情

EQUATION

反应方程式

HRID 743429 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2-(N-carbobenzyloxyaminosulfonyl) aminopentanoic acid methyl ester (33 g) in methanol (250 ml) under nitrogen was cooled to 0° C. and 1.4 g of 10% Pd/C was added. The mixture was placed into a Parr Apparatus and hydrogenated for 2 hours. The catalyst was removed on a pad of CELITE® and the filtrate was concentrated in vacuo and purified by flash silica gel chromatography (50% ethyl acetate in hexane) to afford 13.5 g (76%) of 2-(aminosulfonylamino)pentanoic acid methyl ester (Formula VII: R=CH3 ; R1 =H; R2 =propyl; R3 =H) as a solid, m.p. 63°-64° C.

WORKUP

后处理

  1. customThe catalyst was removed on a pad of CELITE®
  2. concentrationthe filtrate was concentrated in vacuo
  3. custompurified by flash silica gel chromatography (50% ethyl acetate in hexane)