HRID1275713

反应详情

EQUATION

反应方程式

HRID 1275713 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customthe oil that separated off
  2. extractionwas extracted with ethyl acetate
  3. washThe organic phase was washed with 1N hydrochloric acid
  4. customdried
  5. concentrationconcentrated
  6. customa rotary evaporator
  7. customThe crude product was recrystallized from isopropanol