HRID1637985

反应详情

EQUATION

反应方程式

HRID 1637985 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred mixture of 3-(4-methyl-1-piperazinyl)-1-phenylsulfonyl-1H-indazole (13.5 g, 38 mmol), methanol (150 ml) and 25% CH3ONa in methanol (15.3 ml) was stirred and refluxed for 2.5 hours. The reaction was concentrated to about one-tenth its volume, and water was added to the mixture, resulting in a red solution. The solution was extracted with dichloromethane, the extract washed (H2O), dried (MgSO4), and the solvent was concentrated to afford 6.6 g of a rose-colored solid. Two recrystallizations from toluenehexane afforded 4.3 g (52%) of 3-(4-methyl-1-piperazinyl)-1H-indazole as an off-white solid, m.p.=111-113° C.

WORKUP

后处理

  1. temperaturerefluxed for 2.5 hours
  2. concentrationThe reaction was concentrated to about one-tenth its volume, and water
  3. additionwas added to the mixture
  4. customresulting in a red solution
  5. extractionThe solution was extracted with dichloromethane
  6. washthe extract washed (H2O)
  7. dry with materialdried (MgSO4)
  8. concentrationthe solvent was concentrated