HRID1440455

反应详情

EQUATION

反应方程式

HRID 1440455 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of NaOEt (0.217 mol) in EtOH (prepared from 5.0 g of Na and 220 mL of EtOH) was added ethyl trifluoroacetoacetate (40.0 g, 0.217 mol). After 10 min, ethyl 3-bromopropionate (35.0 g, 0.194 mol) was added and the mixture was heated under reflux for 24 h. The reaction mixture was concentrated, taken up in ether, and washed with water. The ether layers were dried (MgSO4) and concentrated to give 50 g of a yellow oil. Distillation (100°-110° C./25 min) gave 14.0 g (23%) of product as a colorless oil.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 24 h
  3. concentrationThe reaction mixture was concentrated
  4. washwashed with water
  5. dry with materialThe ether layers were dried (MgSO4)
  6. concentrationconcentrated