HRID2307349
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A mixture of 1-methyl-4-(4-methylphenyl)-1H-pyrazole (1.70 g), potassium permanganate (9.70 g), and 1 N sodium hydroxide (100 ml) was refluxed for 18 hours. The suspension was filtered through diatomaceous earth and cooled. The aqueous solution was extracted with dichloromethane which was discarded. The aqueous solution was acidified to pH 5.5. The resultant precipitate was difficult to filter and was thus extracted with dichloromethane. After evaporation of the solvent, the resulting solid was recrystallized from acetone to yield the title compound (0.60 g), m.p. 274-275° C.; MS m/z: 202 (M)+.
WORKUP
后处理
- temperaturewas refluxed for 18 hours
- filtrationThe suspension was filtered through diatomaceous earth
- temperaturecooled
- extractionThe aqueous solution was extracted with dichloromethane which
- filtrationto filter
- extractionwas thus extracted with dichloromethane
- customAfter evaporation of the solvent
- customthe resulting solid was recrystallized from acetone