HRID1249296

反应详情

EQUATION

反应方程式

HRID 1249296 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-15 °C

PROCEDURE

实验过程

A solution of 4-(2,4-dinitrophenoxy)-phenyldiazomethane in CH2Cl2 (20 ml) is added to a solution of Boc-dehydroalanine-p-nitrobenzyl ester (2) in 20 ml CH2Cl2 at -15° C. After stirring 1 hr at -15° C. and 4 hr at 25°, the solution is evaporated to dryness and the residue is triturated with hexane. The solid product, p-nitrobenzyl 3-t-butoxycarbonylamino-5-(4-[2,4-dinitrophenoxyl]-phenyl)-pyrazoline-3-carboxylate (18), is recrystallized from ethyl acetate-hexane to constant melting point. NMR (CDCl3)δ: 4.8-5.4 (m, 1H, CH--N=N).

WORKUP

后处理

  1. customthe solution is evaporated to dryness
  2. customthe residue is triturated with hexane
  3. customThe solid product, p-nitrobenzyl 3-t-butoxycarbonylamino-5-(4-[2,4-dinitrophenoxyl]-phenyl)-pyrazoline-3-carboxylate (18), is recrystallized from ethyl acetate-hexane