反应详情

A stream of dry oxygen was passed through a stirred suspension heated at 30° C.) of 1-(2,3-dimethyl-1-phenyl-3-pyrazolin-5-one-4-yl)-2,2,2-trichloroethanol (3,35 g; 10 m. moles) in methanol (15 ml) and a solution of cupric chloride dihydrate (0.025 g; 0.15 m. mole) and 1,10-phenanthroline hydrate 0.075 g; 0.38 m. mole) in methanol (15 ml) in which sodium (0.27 g; 11.7 m. moles) had been dissolved was added portionwise over a period of 60 minutes. The reaction was allowed to proceed for a further 60 minutes, the reaction mixture diluted with dilute sulphuric acid and adjusted to pH 6.0-6.5 by addition of aqueous sodium bicarbonate. The mixture was extracted with chloroform (3×50 ml), the combined extracts washed with saturated aqueous sodium carbonate (10 ml), dried (MgSO4) and evaporated to give methyl 2,3-dimethyl-1-phenyl-3-pyrazolin-5-one-4-carboxylate (2.15 g; 87%). The product was recrystallised from acetone to give material, m.p. 154°-157° C.

1. additionwas added portionwise over a period of 60 minutes
2. extractionThe mixture was extracted with chloroform (3×50 ml)
3. washthe combined extracts washed with saturated aqueous sodium carbonate (10 ml)
4. dry with materialdried (MgSO4)
5. customevaporated