HRID1936768

反应详情

EQUATION

反应方程式

HRID 1936768 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-[2-(Methylsulphonamido)ethyl]acetamide (14.5 g, 88.3 mmol) and concentrated hydrochloric acid (100 ml) were dissolved in water (100 ml) and heated to reflux for a total of 3 hours. After cooling, the water was removed in vacuo, and the residue was left for several days at room temperature until crystallisation was underway. Trituration with a mixture of ethanol and ether gave the title compound as a white solid which was dried in vacuo at 60° C. (7.5 g, 42.9 mmol, 49%); δH [2H6]DMSO 8.22 (2H,br s), 7.42 (1H,t), 3.23 (2H,q), 2.87 (3H,s), 2.85-2.95 (2H,m).

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for a total of 3 hours
  3. temperatureAfter cooling
  4. customthe water was removed in vacuo
  5. waitthe residue was left for several days at room temperature until crystallisation
  6. additionTrituration with a mixture of ethanol and ether