HRID1176955

反应详情

EQUATION

反应方程式

HRID 1176955 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of N,N′-dimethylethylenediamine (25.0 g, 0.28 mol) in 150 mL of dry diethyl ether was added diethyl oxalate (38.5 mL, 0.28 mol) in one portion. After a few minutes white crystals started to precipitate. The reaction mixture was stirred at room temperature overnight. The product was filtered and washed with dry diethyl ether. The product was dried under vacuum at 47° C. overnight to give colorless crystals (38.64 g, 96%). 1H NMR (200 MHz, CDCl3, δ): 3.50 (s, 4H), 2.99 (s, 6H). 13C{1H} NMR (200 MHz, CDCl3, δ): 157.35, 45.91, 34.74.

WORKUP

后处理

  1. waitAfter a few minutes white crystals started
  2. customto precipitate
  3. filtrationThe product was filtered
  4. washwashed with dry diethyl ether
  5. customThe product was dried under vacuum at 47° C. overnight