HRID1637985
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturerefluxed for 2.5 hours
- concentrationThe reaction was concentrated to about one-tenth its volume, and water
- additionwas added to the mixture
- customresulting in a red solution
- extractionThe solution was extracted with dichloromethane
- washthe extract washed (H2O)
- dry with materialdried (MgSO4)
- concentrationthe solvent was concentrated