HRID76114

反应详情

EQUATION

反应方程式

HRID 76114 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 (1-benzyl-5-methoxy-1H-indazol-3-yl)methanol (18 g; 0.07 mol) in chloroform (200 ml) stirred at room temperature was slowly added thionyl chloride (15.8 g; 0.13 mol). Once the addition was complete, the solution was refluxed for 24 hours. The reaction was then stopped by cooling the mixture to room temperature and evaporating off the solvent under reduced pressure. The residue was then taken up several times in toluene and concentrated under reduced pressure. The crude residue obtained was purified by crystallization from hexane to give 9.5 g of 1-benzyl-3-(chloromethyl)-5-methoxy-1H-indazole with a melting point of 78-80° C.

WORKUP

后处理

  1. additionOnce the addition
  2. temperaturethe solution was refluxed for 24 hours
  3. customevaporating off the solvent under reduced pressure
  4. concentrationconcentrated under reduced pressure
  5. customThe crude residue obtained
  6. customwas purified by crystallization from hexane