反应详情

温度

120 °C

Toluene (1.38 g), methanol (32 mg), di-tert-butyl peroxide (73 mg, 1 equivalent), and Pd(Xantphos)Cl2 (3.8 mg, 1 mol %) were added into a reaction kettle, into which 10 atm carbon monoxide was introduced. The reaction was heated to 120° C., and stirred at this constant temperature for 16 h. After the reaction was completed, carbon monoxide was discharged, and 67 mg methyl phenylacetate was obtained by column chromatography, in a yield of 89%. 1HNMR (400 MHz, CDCl3) δ 3.60 (s, 2H), 3.65 (s, 3H), 7.22-7.32 (m, 5H); 13CNMR (100 MHz, CDCl3) δ 41.2, 52.0, 127.1, 128.6, 129.3, 134.1, 172.0; HRMS (ESI) calcd. for C9H10NaO2 [M+Na]: 173.0568. found: 173.0573. The methyl phenylacetate obtained was dissolved in 1,4-dioxane. 6 N sodium hydroxide solution was added, and the reaction was heated to 60° C. After 2 h of reaction, the pH value was adjusted to 1 by adding 2 N hydrochloric acid. After removing the organic solvent under reduced pressure, 58 mg product phenylacetic acid was obtained by extraction with ethyl acetate, and the yield of hydrolysis was 95%.

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