HRID1107686

反应详情

EQUATION

反应方程式

HRID 1107686 的结构方程式

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

21.35 g of phosphorus oxychloride was dropwise added to 4.72 g of DMF at 10° C. or lower. After the temperature of the reaction solution was returned to room temperature, the reaction mixture was stirred for 1 hour, and 10.71 g of 1-methyl-3-trifluoromethyl-5-pyrazolone was added thereto. The resulting mixture was heated up to 110° C., and stirred for 7 hours. After having been left to be at 70° C. the reaction mixture was poured into ice water. After pH of the mixture was made to be about 4 with an aqueous solution of sodium hydroxide added thereto, and precipitated crystals were taken out through filtration and dried to obtain 10.55 g of 1-methyl-3-trifluoromethyl-5-chloropyrazole-4-carbaldehyde.

WORKUP

后处理

  1. customwas returned to room temperature
  2. stirringstirred for 7 hours
  3. waitAfter having been left
  4. customto be at 70° C.
  5. additionadded
  6. customprecipitated crystals
  7. filtrationwere taken out through filtration
  8. customdried