反应详情

To a solution of 3,5-dimethoxy-4-methylbenzaldehyde (3.0 g, 16.8 mmol) in CH2Cl2 (35 mL) was added meta-chloroperoxybenzoic acid (77% purity; 5.8 g, 25.9 mmol). After stirring at room temperature for 19 hrs, additional meta-chloroperoxybenzoic acid (77% purity; 3.5 g, 15.6 mmol) was added. After heating for 4 hrs at 40° C. and cooling to room temperature, 10% aqueous Na2S2O5 was added and the mixture was stirred for 30 min. The mixture was diluted with CH2Cl2 and the layers separated. The organics were washed with 10% aqueous Na2S2O5, ˜5% aqueous NaHCO3 and brine then dried over MgSO4 and concentrated to give 3,5-dimethoxy-4-methylphenyl formate as a yellow solid (2.9 g, 88% yield).

1. temperatureAfter heating for 4 hrs at 40° C.
2. temperaturecooling to room temperature
3. stirringthe mixture was stirred for 30 min
4. customthe layers separated
5. washThe organics were washed with 10% aqueous Na2S2O5, ˜5% aqueous NaHCO3 and brine
6. dry with materialthen dried over MgSO4
7. concentrationconcentrated