HRID133170
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
CONDITIONS
反应条件
- 温度
- 57.5 °C
PROCEDURE
实验过程
104.8 g of 1-(4-methylphenyl)hydrazine hydrochloride are suspended in 525 ml of isopropyl acetate, a solution of 104.8 g of potassium carbonate in 300 ml of water is added and then the mixture is stirred until the solid has disappeared. 77.4 g of acetic anhydride are added while maintaining the temperature below 20° C. and then the mixture is left stirring at 20° C. A precipitate is observed to form, which precipitate disappears when the mixture is heated at approximately 55-60° C. The organic phase is washed twice with 200 ml of water and is then cooled at 0-5° C. overnight. The product formed is recovered by filtration and is then washed twice with 100 ml of MTBE.
WORKUP
后处理
- temperaturewhile maintaining the temperature below 20° C.
- waitthe mixture is left
- stirringstirring at 20° C
- customto form
- customwhich precipitate
- washThe organic phase is washed twice with 200 ml of water
- temperatureis then cooled at 0-5° C. overnight
- customThe product formed
- filtrationis recovered by filtration
- washis then washed twice with 100 ml of MTBE