反应详情

2-(hydroxymethyl)-5-(methylsulfonyl)phenol (3.3 g, 16.3 mmol), 2-bromo-1,1-dimethoxyethane (19.0 ml, 163 mmol), dry THF (30 ml) and concentrated H2SO4 (5 ml) were heated at 55° C. for 1 h. The reaction mixture was brought to ambient temperature and EtOAc and water were added. The phases were separated and the aqueous phase was extracted twice with EtOAc. The combined organic phases were dried (Na2SO4), filtered and evaporated to dryness to give an oil (9.0 g). The oil was crystallizing upon cooling. The product was washed with EtOAc, EtOH and DEE and afforded the pure title compound (4.0 g, 80%). MS m/z (rel. intensity, 70 eV) 308 (M+, 11), 306 (M+, 10), 213 (45), 184 (bp), 77 (35).

1. customwas brought to ambient temperature
2. customThe phases were separated
3. extractionthe aqueous phase was extracted twice with EtOAc
4. dry with materialThe combined organic phases were dried (Na2SO4)
5. filtrationfiltered
6. customevaporated to dryness