反应详情

In 200 ml of chloroform was dissolved 10.0 g of 4-acetoxy-3,5-di-t-butyl-2-(2-methyl-2-propenyl)phenol synthesized in accordance with JP 6-206842 A/94, and 11.0 g of m-chloroperbenzoic acid was added thereto, followed by heating under reflux for one day. After cooling, a saturated aqueous solution of sodium thiosulfate was added to the reaction mixture, and the mixture was extracted with chloroform. The organic layer was washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate, and concentrated. The residue was purified by silica gel column chromatography (25% ethyl acetate in n-hexane) to give 7.3 g (yield: 70%) of 5-acetoxy-4,6-di-t-butyl-2-hydroxymethyl-2-methyl-2,3-dihydrobenzofuran (rotational isomer mixture) as a colorless oil.

1. additionwas added
2. temperatureby heating
3. temperatureunder reflux for one day
4. temperatureAfter cooling
5. extractionthe mixture was extracted with chloroform
6. washThe organic layer was washed with a saturated sodium chloride aqueous solution
7. dry with materialdried over anhydrous magnesium sulfate
8. concentrationconcentrated
9. customThe residue was purified by silica gel column chromatography (25% ethyl acetate in n-hexane)