HRID1792761

反应详情

EQUATION

反应方程式

HRID 1792761 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

4-Nitrobenzenesulphonamide (2.02 g, 10 mmol) was added to a solution of 1,3,5-trioxane (1.96 g, 20 mmol) in acetic acid (5 ml). The mixture was stirred for 5 minutes and methanesulphonic acid (10 ml) was added slowly. The mixture was then stirred at 35° C. for 20 minutes, cooled to 0° C., diluted with water and extracted with ethyl acetate. The combined extracts were washed twice with water and twice with 5% aqueous sodium hydrogen carbonate solution, and then dried and the volatiles removed by evaporation. The residue was recrystallized from ethanol to give the title compound (955 mg, 35% yield). NMR: 4.87 (s, 2H), 5.30 (s, 4H), 8.20 (d, 2H), 8.42 (d, 2H).

WORKUP

后处理

  1. stirringThe mixture was then stirred at 35° C. for 20 minutes
  2. extractionextracted with ethyl acetate
  3. washThe combined extracts were washed twice with water and twice with 5% aqueous sodium hydrogen carbonate solution
  4. customdried
  5. customthe volatiles removed by evaporation
  6. customThe residue was recrystallized from ethanol