HRID1734420

反应详情

EQUATION

反应方程式

HRID 1734420 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.3 g of allyl bromide was added to a mixture comprising 5 g (22 mmol) of 4-hydroxy-2-methyl-2H-indazole-3-sulfonamide and 50 ml of a DMF solution of 1.9 g (22 mmol) of sodium hydrogencarbonate, and the mixture was stirred at room temperature for 12 hours. The mixture was poured into ice water, acidified with citric acid and extracted with ethyl acetate. The organic layer was washed, then concentrated and purified by column chromatography (hexane/ethyl acetate=2/1) to obtain 1.9 g (yield: 32.5%) of the desired product. Melting point: 143°-144° C.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed
  3. concentrationconcentrated
  4. custompurified by column chromatography (hexane/ethyl acetate=2/1)