反应详情

温度

-78 °C

A mixture of 1 mmol of 3,5-dimethoxy-2-(5-methyl-3-methoxy-phenoxy)-4-methyl-benzoic acid methyl ester and 6 mmol of dichloromethyl methyl ether was taken in 8 mL of dichloromethane. The mixture was cooled to −78° C. under stirring, and then titanium tetrachloride (6 mmol) in dichloromethane (4 ml) was added dropwise over 0.5 h. Upon completion, the reaction mixture was poured into ice-cold water and partitioned. The layers were separated, and the aqueous layer was extracted with dichloromethane. The combined organic layers were dried over MgSO4, and the solvent was evaporated by a rotary evaporator. The residue was purified by column chromatography to afford 2-(3-methyl-2-Formyl-5-methoxy-phenoxy)-3,5-dimethoxy-4-methyl-benzoic acid methyl ester (60%).

1. additionUpon completion, the reaction mixture was poured into ice-cold water
2. custompartitioned
3. customThe layers were separated
4. extractionthe aqueous layer was extracted with dichloromethane
5. dry with materialThe combined organic layers were dried over MgSO4
6. customthe solvent was evaporated by a rotary evaporator
7. customThe residue was purified by column chromatography