HRID1159480

反应详情

EQUATION

反应方程式

HRID 1159480 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionThereto was dropwise added, in 0.5 hour
  2. additionAfter the dropwise addition
  3. stirringthe mixture was stirred at room temperature for 1 hour and successively at 80° C. for 5 hours
  4. customto give rise
  5. customto a reaction
  6. customAfter the reaction
  7. temperaturethe mixture was cooled to room temperature
  8. filtrationThe resulting crystals were collected by filtration
  9. washwashed with 50 ml of water twice
  10. customdried in a hot-air drier,