Method for selective oxidation of toluene compounds
A compound and selective technology, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of difficult reaction control, high reaction temperature, poor compatibility, etc., to achieve novel reaction methods, high selectivity, Easy-to-use effects
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Embodiment 1
[0033]In a 100 ml agate ball grinding, 1.37 g (10 mmol) 4-nitr-nitroenzene, 0.0004 g (0.0005 mmol) 5,10,15,20- four (4-chlorophenyl) porphyrin cobalt (II), 2.57 g (20 mmol) 70% T-butyl hydrogen peroxide aqueous solution and 4.11 g of anhydrous sodium sulfate mixed, sealed ball grinding tank. At room temperature, the 600rpm speed under the ball was 0.0h, and the ball milling was stopped every 1.0h, and the gas in the ball mill was released. After completion of the reaction, the resulting reaction mixture was dissolved in 30 ml of anhydrous ethanol, and stirred at room temperature for 30.0 min. Filtration, 2 × 10 ml of anhydrous ethanol washing the resulting filter cake, combined with ethanol solution, and disposable to 100 ml of the obtained ethanol solution. 10 ml of the resulting solution was removed, and the internal standard 2-naphthoic acid was added to perform liquid chromatography. 4-Nitrotrosenzene conversion rate of 11%, 4-nitrophenate selectivity 99%, no other obvious oxi...
Embodiment 2
[0035] In a 100 ml agate ball grinding, 1.37 g (10 mmol) 4-nitr-nitroenzene, 0.0020 g (0.0025 mmol) 5,10,15,20- 4 (4-chlorophenyl) porphyrin cobalt (II), 2.57g (20 mmol) 70% T-butyl hydrogen peroxide aqueous solution and 4.11 g of anhydrous sodium sulfate mixed, sealed ball grinding tank. At room temperature, the 600rpm speed under the ball was 0.0h, and the ball milling was stopped every 1.0h, and the gas in the ball mill was released. After completion of the reaction, the resulting reaction mixture was dissolved in 30 ml of anhydrous ethanol, and stirred at room temperature for 30.0 min. Filtration, 2 × 10 ml of anhydrous ethanol washing the resulting filter cake, combined with ethanol solution, and disposable to 100 ml of the obtained ethanol solution. 10 ml of the resulting solution was removed, and the internal standard 2-naphthoic acid was added to perform liquid chromatography. 4-Nitrotrosenzene conversion rate of 14%, 4-nitrophenate selectivity 99%, no other obvious oxidat...
Embodiment 3
[0037] In a 100 ml agate ball grinding, 1.37 g (10 mmol) 4-nitrotropylbenzene, 0.0008 g (0.0010 mmol) 5,10,15,20- (4-chlorophenyl) porphyrin cobalt (II), 2.57 g (20 mmol) 70% T-butyl hydrogen peroxide aqueous solution and 4.11 g of anhydrous sodium sulfate mixed, sealed ball grinding tank. At room temperature, the 600rpm speed under the ball was 0.0h, and the ball milling was stopped every 1.0h, and the gas in the ball mill was released. After completion of the reaction, the resulting reaction mixture was dissolved in 30 ml of anhydrous ethanol, and stirred at room temperature for 30.0 min. Filtration, 2 × 10 ml of anhydrous ethanol washing the resulting filter cake, combined with ethanol solution, and disposable to 100 ml of the obtained ethanol solution. 10 ml of the resulting solution was removed, and the internal standard 2-naphthoic acid was added to perform liquid chromatography. 4-Nitrotrosenzene conversion of 12%, 4-nitrophenylbenzoic acid selectivity 99%, and other obviou...
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