Methyl iodide → HCID 22940168, compound

In acetone (30 mL) was dissolved 2.00 g (11.2 mmol) of 1-(2-hydroxy-3,4,6-trimethylphenyl)ethanone which can be produced by the method disclosed in Chemical Research in Toxicology, 1997, vol. 10, No. 3, pp. 335-343, 3.10 g (22.4 mmol) of potassium carbonate, then 1.40 mL (22.5 mmol) of methyl iodide were added to the solution, and the resulting mixture was refluxed for 5 hours. After cooling to room temperature, the reaction mixture was concentrated, and the residue was poured into water, and extracted with ethyl acetate. The organic layers were combined, washed successively with water and brine, and dried over anhydrous magnesium sulfate. The solvent was removed, and the residue was purified by silica gel column chromatography (Wako gel C-100, hexane:ethyl acetate gradient) to obtain 1.90 g (9.90 mmol, Yield: 88.4%) of 1-(2-methoxy-3,4,6-trimethylphenyl)ethanone.

1. customcan be produced by the method
2. temperaturethe resulting mixture was refluxed for 5 hours
3. concentrationthe reaction mixture was concentrated
4. additionthe residue was poured into water
5. extractionextracted with ethyl acetate
6. washwashed successively with water and brine
7. dry with materialdried over anhydrous magnesium sulfate
8. customThe solvent was removed
9. customthe residue was purified by silica gel column chromatography (Wako gel C-100, hexane:ethyl acetate gradient)

ORD record

ord-e2d0dbf0c47f4a82b14482e1dcadd821

Source dataset

uspto-grants-2009_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07608563B2