HRID382796

反应详情

EQUATION

反应方程式

HRID 382796 的结构方程式

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

29 Grams of 3-methyl-1-phenyl-2-pyrazoline-5-one and 40 ml of dimethylformamide were charged into a 200-ml three-necked flask, stirred and cooled to 0° C. in an ice-acetone bath. Then, 18.5 g of phosphorus oxychloride (POCl3) was placed in a dropping funnel, and while it was maintained at 10 to 20° C., it was dropwise added. After the addition, the mixture was heated for 1 hour, then, a reaction mixture was poured into 600 ml of ice water, and the mixture was allowed to stand for one day and night. A crystal was recovered by suction filtration, fully washed with water and dried to give the captioned compound. Yield: 65%, Melting point: 178-180° C. (documented value: 174-175° C.).

WORKUP

后处理

  1. temperaturewhile it was maintained at 10 to 20° C.
  2. additionit was dropwise added
  3. additionAfter the addition
  4. temperaturethe mixture was heated for 1 hour
  5. filtrationA crystal was recovered by suction filtration
  6. washfully washed with water
  7. customdried
  8. customto give the captioned compound
  9. customYield: 65%, Melting point: 178-180° C. (documented value: 174-175° C.)