HRID64830

反应详情

EQUATION

反应方程式

HRID 64830 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To an ethyl acetate solution of Nα -benzyloxycarbonyl-L-histidinazide (4) prepared from Nα -benzyloxycarbonyl-L-histidine hydrazide (3) (6.07 g) by a known method was added 10 ml of a DMF solution of 2.31 g of (S)-N-(2-hydroxyethyl)-2-pyrrolidinecarboxamide (53) under ice-cooling and they were reacted overnight in a refrigerator. The reaction mixture was concentrated and the residue thus formed was subjected to silica gel column chromatography. By eluting the product with chloroform-methanol-aqueous ammonia (90:10:1), 3.43 g of Nα -benzyloxycarbonyl-L-histidyl-N-(2-hydroxyethyl)-L-prolinamide (54) was obtained.

WORKUP

后处理

  1. temperaturecooling
  2. customthey were reacted overnight in a refrigerator
  3. concentrationThe reaction mixture was concentrated
  4. customthe residue thus formed
  5. washBy eluting the product with chloroform-methanol-aqueous ammonia (90:10:1)