HRID1648304

反应详情

EQUATION

反应方程式

HRID 1648304 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Diethyl (formylamino)malonate (20.3 g, 0.1 mol) was added to a stirred solution of sodium ethoxide (250 mL of 0.4 M). 2-Nitrobenzyl chloride (17.2 g, 0.1 mol) was added, the mixture was refluxed for 2 hours and the solvent was then removed under reduced pressure. The material was partitioned between ethyl acetate and water, the ethyl acetate was separated and evaporated to give 40.3 g of crude product. The compound was crystallized from ethyl acetate:hexane to give 25.5 g of diethyl (formylamino)((2-nitrophenyl)methyl)propanedioate; mp 129°-132° C.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 2 hours
  2. customthe solvent was then removed under reduced pressure
  3. customThe material was partitioned between ethyl acetate and water
  4. customthe ethyl acetate was separated
  5. customevaporated
  6. customto give 40.3 g of crude product
  7. customThe compound was crystallized from ethyl acetate