反应详情

温度

90 °C

1,8-diazabicyclo[5.4.0]undec-7-ene (DBU), (836 mg, 5.49 mmol), was added to a mixture of 2,6-dimethoxybenzoic acid (1), (1.0 g, 5.49 mmol), in dimethyl carbonate (DMC) (10 mL) and the resulting mixture was heated to reflux at 90° C. for 4 hours. The reaction mixture was cooled to 25° C. and diluted with EtOAc (30 mL) and water (30 mL). The organic layer was separated and washed in sequence with 10 mL of water, 2 M HCl (2×30 mL), saturated aqueous NaHCO3 (2×30 mL) and water (2×25 mL). The organic layer was dried over Na2SO4, filtered and concentrated under vacuum to give methyl 2,6-dimethoxybenzoate (2) as a white solid. The yield of the 2,6-dimethoxybenzoate as determined by HPLC was 97-98% conversion.

1. temperaturethe resulting mixture was heated
2. temperatureThe reaction mixture was cooled to 25° C.
3. customThe organic layer was separated
4. washwashed in sequence with 10 mL of water, 2 M HCl (2×30 mL), saturated aqueous NaHCO3 (2×30 mL) and water (2×25 mL)
5. dry with materialThe organic layer was dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated under vacuum