HRID1594250

反应详情

EQUATION

反应方程式

HRID 1594250 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.06 g (54.6 mmol) of lithium aluminum hydride were initially charged in 250 ml of absolute THF, and a solution of 18.8 g (54.6 mmol) of 1-benzyl-3-(5-ethoxycarbonyl-2-furyl)indazole in 250 ml of THF was added dropwise. After 45 min the mixture was admixed with 25% strength potassium carbonate solution and stirred at RT for 30 min and the precipitate was filtered off with suction and washed with THF. The combined organic phases were concentrated using a rotary evaporator and the residue was recrystallized from isopropanol. This gave 11.0 g (67%) of the title compound. m.p.: 113-114° C.

WORKUP

后处理

  1. filtrationthe precipitate was filtered off with suction
  2. washwashed with THF
  3. concentrationThe combined organic phases were concentrated
  4. customa rotary evaporator
  5. customthe residue was recrystallized from isopropanol