HRID1278044

反应详情

EQUATION

反应方程式

HRID 1278044 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Add a solution of 2.35 g of potassium tert. butylate in 15 ml of tert. butanol and 10 ml of dimethylformamide dropwise at 130° to a mixture of 5.0 g of 2-dimethylamino-1-methyl-1-pyrrolinium methylsulfate and 2.2 g of 4-nitrotoluene in 15 ml of dimethylformamide. Stir the thus-prepared reaction mixture at this temperature for 2 hours. Allow the mixture to cool, add water to it and then extract it several times with chloroform. Combine and then concentrate the chloroform extracts. Distil off a slight excess of 4-nitrotoluene under a high vacuum and recrystallize the produced residue from 10 ml of ethanol to obtain 0.8 g of title compound.

WORKUP

后处理

  1. customthe thus-prepared reaction mixture at this temperature for 2 hours
  2. temperatureAllow the mixture to cool
  3. extractionextract it several times with chloroform
  4. concentrationCombine and then concentrate the chloroform
  5. customDistil off a slight excess of 4-nitrotoluene under a high vacuum
  6. customrecrystallize the produced residue from 10 ml of ethanol