HRID1440456

反应详情

EQUATION

反应方程式

HRID 1440456 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 (0.026 mol) in EtOH (prepared from 0.60 g of Na and 30 mL of EtOH) was added diethyl trifluoroacetylglutarate (3.70 g, 0.013 mol) and acetamidine hydrochloride (1.23 g, 0.013 mol). The reaction mixture was heated under reflux for 18 h , concentrated, and taken up in water. The mixture was acidified to pH 4 with 2N HCl and extracted with CH2Cl2. The extracts were dried (MgSO4) and concentrated to give a yellow solid. Trituration with hexane gave 0.87 g of product as a white solid.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureunder reflux for 18 h
  3. concentrationconcentrated
  4. extractionextracted with CH2Cl2
  5. dry with materialThe extracts were dried (MgSO4)
  6. concentrationconcentrated
  7. customto give a yellow solid