HRID382796
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperaturewhile it was maintained at 10 to 20° C.
- additionit was dropwise added
- additionAfter the addition
- temperaturethe mixture was heated for 1 hour
- filtrationA crystal was recovered by suction filtration
- washfully washed with water
- customdried
- customto give the captioned compound
- customYield: 65%, Melting point: 178-180° C. (documented value: 174-175° C.)