HRID370704

反应详情

EQUATION

反应方程式

HRID 370704 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

20.7 g of 5-aminobenzotriazole dihydrochloride and 30 g of sodium hydrogen carbonate were dissolved in 300 ml of water, and 10 g of acryl chloride was added dropwise at a temperature of lower than 10° C. over 20 minutes. After being stirred for 1 hour, the formed white precipitate was filtered off. Yield: 13.8 g. It was dissolved in 100 ml of DMF, and 500 ml of hot water at about 70° C. was added. It was immediately filtered under atmospheric pressure. The filtrate was allowed to cool, and the separated crystals were filtered out, washed with water and dried to obtain 11 g of the desired product which melted at 248°-253° C. The structure was confirmed by IR, NMR and elementary analysis.

WORKUP

后处理

  1. filtrationthe formed white precipitate was filtered off
  2. dissolutionIt was dissolved in 100 ml of DMF
  3. addition500 ml of hot water at about 70° C. was added
  4. filtrationIt was immediately filtered under atmospheric pressure
  5. temperatureto cool
  6. filtrationthe separated crystals were filtered out
  7. washwashed with water
  8. customdried