HRID76115

反应详情

EQUATION

反应方程式

HRID 76115 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 the crude isobutyl 1-tritylindazole-3-carboxylate (180 g; 0.39 mol) in THF (1 L) stirred at room temperature was added slowly a suspension of LiAlH4 (18 g; 0.48 mol) in THF (100 ml). Once the addition was complete, the mixture was stirred at room temperature for 30 minutes, and the reaction was then stopped by cooling the mixture to 0° C. and successively adding water (40 ml), 2N NaOH (40 ml) and water (60 ml). The solid thus formed was filtered off and the solution was concentrated under reduced pressure. The crude residue obtained was purified by crystallization from a 1/1 hexane/ethyl acetate mixture. 120 g of (1-tritylindazol-3-yl)methanol were obtained.

WORKUP

后处理

  1. additionwas added slowly
  2. additionOnce the addition
  3. temperatureby cooling the mixture to 0° C.
  4. customThe solid thus formed
  5. filtrationwas filtered off
  6. concentrationthe solution was concentrated under reduced pressure
  7. customThe crude residue obtained
  8. customwas purified by crystallization from a 1/1 hexane/ethyl acetate mixture