反应详情

To a mixture of 3-methyl-salicylic acid (1.32 mol)and anhydrous potassium carbonate (3.6 mol)dissolved in 3.5 L of dry acetone in a 5L round bottle flask, dimethylsulfate (2.2 mol) was added in several times. The mixture was refluxed overnight, and the reaction was monitored by TLC. After filtration of the reaction mixture, the solvents of the filtrate were evaporated and 215 g of a pale yellow thick oil was obtained as the raw product. Yield 91%. 1H NMR (500 MHz, CDCl3, 25° C.) δ: 2.263 (s, 3H, CH3), 3.782 (s, 3H, OCH3), 3.854 (s, 3H, OCH3), 6.984 (t, J=7.5, 1H, ArH), 7.276 (d, J=7.5, 1H, ArH), 7.582 (d, J=7.5, 1H, ArH); 13C NMR (500 MHz, CDCl3, 25° C.) δ: 15.72, 51.81, 61.17, 123.26, 124.36, 128.86, 132.46, 134.88, 158.16, 166.61.

1. additionwas added in several times
2. temperatureThe mixture was refluxed overnight
3. filtrationAfter filtration of the reaction mixture
4. customthe solvents of the filtrate were evaporated