HRID1907134

反应详情

EQUATION

反应方程式

HRID 1907134 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-methyl-1,6-dihydro-pyrrolo[2,3-g]indazole-7,8-dione (23 g, 114.3 mmol) in 4N aqueous sodium hydroxide solution (160 ml) at ambient temperature, was added dropwise 30% aqueous hydrogen peroxide solution (27 ml) maintaining the temperature <30° C. with external cooling. The resulting reaction mixture was stirred at ambient temperature for 2 hours. According to TLC, the reaction was complete after 2 hours. The pH was adjusted to pH 3.5 by addition of concentrated hydrochloric acid. The resulting brown suspension was filtered and the filtercake washed with cold water and dried in vacuo at 50° C. to afford the desired product as brown solid. LC/MS: 192 (M+H)+.

WORKUP

后处理

  1. temperaturemaintaining the temperature <30° C. with external cooling
  2. customThe resulting reaction mixture
  3. waitthe reaction was complete after 2 hours
  4. filtrationThe resulting brown suspension was filtered
  5. washthe filtercake washed with cold water
  6. customdried in vacuo at 50° C.