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
- 10 °C
PROCEDURE
实验过程
18.4 g (0.1 mole) of ethyl 4,4,4-trifluoroacetoacetate was dissolved in 12.0 g (0.2 mole) of acetic acid. The solution was cooled to 10° C. or lower with stirring. Thereto was dropwise added, in 0.5 hour, 11.8 g (0.11 mole) of phenylhydrazine. After the dropwise addition, the mixture was stirred at room temperature for 1 hour and successively at 80° C. for 5 hours to give rise to a reaction. After the reaction, the mixture was cooled to room temperature. Thereto were added 100 ml of water. The resulting crystals were collected by filtration, washed with 50 ml of water twice, and dried in a hot-air drier, to obtain 22.3 g (yield: 98.0%) of a title compound as light yellow crystals.
WORKUP
后处理
- additionThereto was dropwise added, in 0.5 hour
- additionAfter the dropwise addition
- stirringthe mixture was stirred at room temperature for 1 hour and successively at 80° C. for 5 hours
- customto give rise
- customto a reaction
- customAfter the reaction
- temperaturethe mixture was cooled to room temperature
- filtrationThe resulting crystals were collected by filtration
- washwashed with 50 ml of water twice
- customdried in a hot-air drier,