Water → HCID 18629335, compound

Temperature

90 °C

5.49 g of 5-bromo-2,3-dimethylphenol (3-17) was dissolved in 100 ml of DMF, to which were added 6.80 g of methyl iodide and 11.32 g of potassium carbonate, and the resulting mixture was stirred at 90° C. for 2 hours. The reaction solution was poured into water, and extracted with ethyl acetate and the resulting organic layer was washed with saturated salt water, and thereafter, the resulting organic layer was dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the resulting residue was purified by silica gel column chromatography (eluent; hexane:ethyl acetate=9:1) to obtain 5.35 g of 5-bromo-1-methoxy-2,3-dimethylbenzene (3-18).

1. extractionextracted with ethyl acetate
2. washthe resulting organic layer was washed with saturated salt water
3. dry with materialthe resulting organic layer was dried over anhydrous magnesium sulfate
4. customThe solvent was removed under reduced pressure
5. customthe resulting residue was purified by silica gel column chromatography (eluent; hexane:ethyl acetate=9:1)

ORD record

ord-e3960f3a44734f609470afe5ebefafef

Source dataset

uspto-grants-2003_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06525066B2