反应详情

Carbon tetrachloride (30.3 g, 198 mmol) was added dropwise over 20 minutes to a solution of 3-(4-methxytetrahydropyran-4-yl)benzyl alcohol from Step 4 (29.3 g, 132 mmol) and HMPA (32.2 g, 198 mmol) in THF (400 mL) at 0°-5° C. The mixture was stirred for 10 minutes and then concentrated. Excess Et2O was added and the mixture filtered through a celite pad. The filtrate was concentrated and chromatographed on silica gel using 20% EtOAc in hexane as eluent to obtain 24 g (81%) of the title compound as an oil.

1. concentrationconcentrated
2. additionExcess Et2O was added
3. filtrationthe mixture filtered through a celite pad
4. concentrationThe filtrate was concentrated
5. customchromatographed on silica gel using 20% EtOAc in hexane as eluent