HRID76113

反应详情

EQUATION

反应方程式

HRID 76113 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of benzyl 1-benzyl-5-methoxy-1H-indazole-3-carboxylate (17.7 g; 0.05 mol), diethyl ether (100 ml) and tetrahydrofuran (THF) (170 ml) stirred at room temperature was slowly added LiAlH4 (3.8 g; 0.1 mol). Once the addition was complete, the suspension was stirred at reflux for 24 hours. The reaction was stopped by destroying the excess LiAlH4 via addition of water (40 ml) and 5N NaOH (10 ml). The organic phase was separated out and the solvent was evaporated off under reduced pressure. The crude residue obtained was purified by crystallization from 95° ethanol to give 14 g of (1-benzyl-5-methoxy-1H-indazol-3-yl)methanol with a melting point of 97-98° C.

WORKUP

后处理

  1. additionOnce the addition
  2. temperatureat reflux for 24 hours
  3. customby destroying the excess LiAlH4
  4. additionvia addition of water (40 ml) and 5N NaOH (10 ml)
  5. customThe organic phase was separated out
  6. customthe solvent was evaporated off under reduced pressure
  7. customThe crude residue obtained
  8. customwas purified by crystallization from 95° ethanol