反应详情

N-Chlorosulfonyl isocyanate (3.43 mL, 39.4 mmol) was added to a warm solution of 4-(tert-butyl-dimethyl-silanyloxy)-2,6-diisopropylphenol (11.59 g, 37.6 mmol) in 400 mL toluene. The resulting solution was heated to reflux for 6 hours and then cooled to room temperature and stirred overnight. The reaction was concentrated in vacuo, and the residue was quenched with ice water and extracted with dichloromethane. The organic layer was dried over magnesium sulfate, filtered, and concentrated to give an orange oil. Chromatography on silica gel gave 6.06 g of 4-(tert-butyl-dimethyl-silanyloxy)-2,6-diisopropylphenyl sulfamate as an orange oil.

1. temperatureThe resulting solution was heated
2. temperatureto reflux for 6 hours
3. concentrationThe reaction was concentrated in vacuo
4. customthe residue was quenched with ice water
5. extractionextracted with dichloromethane
6. dry with materialThe organic layer was dried over magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated
9. customto give an orange oil