反应详情

A mixture of 4-chloro-3′-methylbiphenyl-3-carboxylic acid (1.70 g, 6.90 mmol), K2CO3 (7.0 g, 50.6 mmol) and CH3I (3 mL, 48 mmol) in acetone (30 mL) was heated under reflux for 1 h. After filtration and evaporation of excess CH3I, the residue was washed with water and extracted with ethyl acetate, dried over anhydrous Na2SO4, and evaporated solvent in vacuo to provide crude methyl 4-chloro-3′-methylbiphenyl-3-carboxylate (1.77 g, 98%) as a brown oil. 1H NMR (300 MHz, DMSO-d6): δ 8.04 (s, 1H), 7.85 (d, J=7.8 Hz, 1H), 7.64 (d, J=8.1 Hz, 1H), 7.52-7.47 (m, 2H), 7.38 (t, J=7.8 Hz, 1H), 7.23 (d, J=7.5 Hz, 1H), 3.90 (s, 3H), 2.39 (s, 3H).

1. temperaturewas heated
2. temperatureunder reflux for 1 h
3. filtrationAfter filtration and evaporation of excess CH3I
4. washthe residue was washed with water
5. extractionextracted with ethyl acetate
6. dry with materialdried over anhydrous Na2SO4
7. customevaporated solvent in vacuo