HRID1883624

反应详情

EQUATION

反应方程式

HRID 1883624 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

7.46 g (23.9 mmol) of 4-(5-bromo-2-methylbenzyl)-5-hydroxymethyl-2-methyl-2,4-dihydro-3H-1,2,4-triazol-3-one and 15.8 g of active manganese dioxide were stirred for 3 hours in nitrogen atmosphere under reflux with heating in 71 ml of chloroform. The reaction solution was filtrated through celite, and the filtrate was concentrated. The residue was subjected to silica gel column chromatography (eluant: hexane/ethyl acetate-1/2 (v/v)), to obtain 5.04 g (16.3 mmol) of 4-(5-bromo-2-methylbenzyl)-5-formyl-2-methyl-2,4-dihydro-3H-1,2, 4-triazol-3-one having a melting point of 107.5° C.

WORKUP

后处理

  1. temperatureunder reflux
  2. filtrationThe reaction solution was filtrated through celite
  3. concentrationthe filtrate was concentrated