A method for preparing carboxylic acid compounds by oxidatively cleaving carbon-carbon bonds of ketone compounds
A ketone compound, oxidative cleavage technology, applied in the field of organic carboxylic acids, can solve the problems of narrow substrate range, harsh reaction conditions, insufficient green oxidant, etc., and achieve the effects of high selectivity, less by-products, and widened substrate range.
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Embodiment 1
[0054] In a 15mL reaction kettle with polytetrafluoroethylene lining, add 0.5mmol acetophenone, weigh 0.1mmol cuprous chloride as a catalyst, and add 2mL solvent acetonitrile (the concentration of acetophenone is 0.25mol / L), and oxygenate Pressure to 0.6MPa, temperature raised to 120°C, stirred and reacted for 10h, after the reaction, gas chromatography-mass spectrometry detected the product, product benzoic acid mass spectrum and standard mass spectrum Figure 1 Sincerely. Gas chromatography quantitative substrate acetophenone conversion rate and product benzoic acid yield are shown in Table 1.
Embodiment 2
[0056] In a 15mL reaction kettle with polytetrafluoroethylene lining, add 0.5mmol acetophenone, weigh 0.1mmol copper acetate as a catalyst, and add 2mL solvent acetonitrile (the concentration of acetophenone is 0.25mol / L), and aerate the pressure with oxygen to 0.6MPa, heat up to 120°C, stir and react for 10h, after the reaction, detect the product by gas chromatography-mass spectrometry, the mass spectrum of the product benzoic acid and the standard mass spectrum Figure 1 Sincerely. Gas chromatography quantitative substrate acetophenone conversion rate and product benzoic acid yield are shown in Table 1.
Embodiment 3
[0058] In a 15mL reaction kettle with a Teflon lining, add 0.5mmol acetophenone, weigh 0.1mmol copper chloride as a catalyst, then add 0.2mmol sodium nitrate as a catalytic promoter, add 2mL solvent acetonitrile (the concentration of acetophenone 0.25mol / L), oxygenated to 0.6MPa, heated to 120°C, and stirred for 10 hours. After the reaction, the product was detected by gas chromatography-mass spectrometry, and the product benzoic acid mass spectrum and standard mass spectrum Figure 1 Sincerely. Gas chromatography quantitative substrate acetophenone conversion rate and product benzoic acid yield are shown in Table 1.
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