HRID1886065

反应详情

EQUATION

反应方程式

HRID 1886065 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