Preparation method of 2-(2'-methyl phenyl)-2-carbonyl acetic acid
A kind of technology of methyl phenyl and carbonyl acetic acid, applied in the field of preparation of 2--2-carbonyl acetic acid, can solve problems such as low yield
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Embodiment 1
[0010] Embodiment 1: the synthesis of 2-(2'-methylphenyl)-2-oxoacetic acid (compound I)
[0011]
[0012] At 0°C to 5°C, add 20mL of water, 2g (50mmol) of sodium hydroxide, 10g (75mmol) of o-methyl acetophenone and 0.48g (1.5mmol) of tetrabutylammonium bromide into a 500mL three-neck round bottom flask, Under stirring, 23.7g (150mmol) of potassium permanganate ground into powder was added to the reaction flask in batches, stirred and reacted at 0°C to 5°C for 1h, and then stirred and reacted at 30°C for 6h. Adjust the pH with concentrated sulfuric acid until no white solid is produced, filter with suction, extract the filtrate with ethyl acetate, combine the organic layers, dry with anhydrous sodium sulfate, and rotary evaporate to obtain 2-(2'-methylphenyl)-2-carbonyl Acetic acid (compound I), yield 90%. NMR data ( 1 HNMR, 400MHz, internal standard TMS, solvent CDCl 3 ) as follows: δppm2.61 (s, 3H, CH3), 7.26-7.69 (m, 4H, ArH), 9.12 (s, 1H, COOH).
Embodiment 2
[0013] Embodiment 2: the synthesis of 2-(2'-methylphenyl)-2-oxoacetic acid (compound I)
[0014]
[0015] At 5°C to 10°C, add 20mL of water, 2g (50mmol) of sodium hydroxide, 10g (75mmol) of o-methyl acetophenone and 0.51g (1.5mmol) of tetrabutylammonium bisulfate into a 500mL three-neck round bottom flask, Under stirring, 23.7g (150mmol) of potassium permanganate ground into powder was added to the reaction flask in batches, stirred and reacted at 5°C to 10°C for 1h, and then stirred and reacted at 30°C for 6h. Adjust the pH with concentrated sulfuric acid until no white solid is produced, filter with suction, extract the filtrate with ethyl acetate, combine the organic layers, dry with anhydrous sodium sulfate, and rotary evaporate to obtain 2-(2'-methylphenyl)-2-carbonyl Acetic acid (compound I), yield 85%.
Embodiment 3
[0016] Embodiment 3: the synthesis of 2-(2'-methylphenyl)-2-oxoacetic acid (compound I)
[0017]
[0018] At 0°C to 5°C, add 20mL of water, 2g (50mmol) of sodium hydroxide, 13.4g (100mmol) of o-methylacetophenone and 0.64g (2mmol) of tetrabutylammonium bromide into a 500mL three-neck round bottom flask, Under stirring, 31.6 g (200 mmol) of potassium permanganate ground into powder was added to the reaction flask in batches, stirred and reacted at 0° C. to 5° C. for 2 h, and then stirred and reacted at 25° C. for 12 h. Adjust the pH with concentrated sulfuric acid until no white solid is produced, filter with suction, extract the filtrate with ethyl acetate, combine the organic layers, dry with anhydrous sodium sulfate, and rotary evaporate to obtain 2-(2'-methylphenyl)-2-carbonyl Acetic acid (compound I), yield 80%.
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