反应详情

Methyl magnesium bromide (2.4 mL, 1.2 eq) was dropwise added at −78° C. to a solution of 2,5-dimethyl-4-methoxybenzaldehyde (1.0 g, 6.0 mmol) in 30 mL of tetrahydrofuran (THF) with stirring and the reaction mixture was allowed to react at that temperature while being stirred. After completion of the reaction, the reaction mixture was adjusted to pH 7 at 0° C. with 1N-HCl and concentrated in a vacuum. The residue thus obtained was stirred in water (20 mL) and extracted twice with 20 mL of dichloromethane. The organic layer was dried over anhydrous magnesium sulfate, filtrated and concentrated in a vacuum to remove the solvent. The concentrate was purified through silica gel chromatography to yield 1-(4-methoxy-2,5-dimethylphenyl)ethanol as a white oil (0.87 g, yield 74%).

1. customto react at that temperature
2. stirringwhile being stirred
3. customAfter completion of the reaction
4. concentrationconcentrated in a vacuum
5. customThe residue thus obtained
6. extractionextracted twice with 20 mL of dichloromethane
7. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
8. filtrationfiltrated
9. concentrationconcentrated in a vacuum
10. customto remove the solvent
11. customThe concentrate was purified through silica gel chromatography