HRID370704
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationthe formed white precipitate was filtered off
- dissolutionIt was dissolved in 100 ml of DMF
- addition500 ml of hot water at about 70° C. was added
- filtrationIt was immediately filtered under atmospheric pressure
- temperatureto cool
- filtrationthe separated crystals were filtered out
- washwashed with water
- customdried