HRID2306695
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureheated
- temperatureto reflux for a total of 3 hours
- temperatureAfter cooling
- customthe water was removed in vacuo
- waitthe residue was left for several days at room temperature until crystallisation
- additionTrituration with a mixture of ethanol and ether