反应详情

The 4-acetoxy-3,5-di-tert-butylanisole obtained in Example 13 and 1.37 kg (9.14 mol) of sodium iodide were dissolved in 5.0 L of acetonitrile; thereafter, 1.16 L (9.14 mol) of trimethylsilyl chloride was added dropwise and the mixture was refluxed for 8 hours. Thereafter, the reaction mixture was cooled to room temperature, water was added and the organic layer was separated. The organic layer was washed with an aqueous solution of sodium thiosulfate and aqueous sodium chloride in that order and dried over anhydrous sodium sulfate. The crude product obtained by concentrating the organic layer was recrystallized from an ethanol/water mixed solvent and the crystal was dried to give 1.55 kg of the title compound (92.4% in yield from the 2,6-di-tert-butyl-4-methoxyphenol of Example 13).

1. temperaturethe mixture was refluxed for 8 hours
2. customthe organic layer was separated
3. washThe organic layer was washed with an aqueous solution of sodium thiosulfate and aqueous sodium chloride in that order
4. dry with materialdried over anhydrous sodium sulfate
5. customThe crude product obtained
6. concentrationby concentrating the organic layer
7. customwas recrystallized from an ethanol/water mixed solvent
8. customthe crystal was dried