HRID1275713
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
2.97 ml (5.94 mmol) of a 2M solution of methylamine in THF were initially charged in 20 ml of THF, and a solution of 0.8 g (2.4 mmol) of 1-benzyl-3-(5-chlorocarbonyl-2-furyl)indazole in 10 ml of THF was added dropwise at RT. After 1 h, the mixture was poured into ice-water and the oil that separated off was extracted with ethyl acetate. The organic phase was washed with 1N hydrochloric acid, dried and concentrated using a rotary evaporator. The crude product was recrystallized from isopropanol. This gave 0.44 g (55%) of the title compound. m.p.: 182-183° C.
WORKUP
后处理
- customthe oil that separated off
- extractionwas extracted with ethyl acetate
- washThe organic phase was washed with 1N hydrochloric acid
- customdried
- concentrationconcentrated
- customa rotary evaporator
- customThe crude product was recrystallized from isopropanol