HRID1594264

反应详情

EQUATION

反应方程式

HRID 1594264 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 2 M 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 1 N 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 1 N hydrochloric acid
  4. customdried
  5. concentrationconcentrated
  6. customa rotary evaporator
  7. customThe crude product was recrystallized from isopropanol