HRID54982

反应详情

EQUATION

反应方程式

HRID 54982 的结构方程式

CONDITIONS

反应条件

温度
35 °C

PROCEDURE

实验过程

To a solution of 2-methyl-4-(4-methylthiophenyl)-1-(2H)-phthalazinone (14.15 g, 0.05 mol) in acetic acid (330 mL) was added 30% H2O2 (22 mL). The mixture was heated to 35° C. overnight, additional 30% H2O2 (10 mL) was added and the mixture was stirred at 35° C. for 2 hours and finally one final portion of 30% H2O2 (10 mL) was added and the mixture was stirred for another 2 hours at 35° C. The reaction mixture was poured into water (1 L)/ice and the solid thus obtained was collected by filtration, washed with water, then ether, and then was dried to afford 14.6 g (93%) of 2-methyl-4-(4-methylsulfonylphenyl)-1-(2H)-phthalazinone as a pale yellow solid, m.p. 218°-220° C. when recrystallized from ethanol/chloroform (2×).

WORKUP

后处理

  1. stirringthe mixture was stirred for another 2 hours at 35° C
  2. customthe solid thus obtained
  3. filtrationwas collected by filtration
  4. washwashed with water
  5. dry with materialether, and then was dried