反应详情

Sodium hydride (60% dispersion in mineral oil, 145 mg) was added portionwise to a solution of 4-(2-hydroxyethyl)phenol (502 mg) in THF (15 ml) and the mixture was stirred at 20° C. for 30 min. tert-Butyldimethylsilyl chloride (547 mg) was added and the mixture was stirred for 75 min. Phosphate buffer solution (pH 6.5) was added and the mixture was extracted with EtOAc. The combined extracts were dried (Na2SO4) and the solvent evaporated in vacuo to give a residue which was purified by SPE (10 g). Elution with DCM-cyclohexane (1:3) then DCM then EtOAc gave the title compound (658 mg). LCMS RT=3.62 min.

1. additionwas added
2. extractionthe mixture was extracted with EtOAc
3. dry with materialThe combined extracts were dried (Na2SO4)
4. customthe solvent evaporated in vacuo
5. customto give a residue which
6. customwas purified by SPE (10 g)
7. washElution with DCM-cyclohexane (1:3)