反应详情

温度

25 °C

459 mg (1.64 mmol equivalents) of 5-benzyloxyethyl-2,2-dimethyl-5-hydroxymethyl-1,3-dioxane was dissolved in 8 mL of dimethylformamide, 197 mg (3.20 mmol equivalents) of imidazole and 0.51 mL (1.92 mmol equivalents) of t-butyldiphenylchlorosilane were added thereto, and the mixture was stirred at room temperature (25° C.) for 22 hours. After completion of the reaction, a saturated aqueous solution of ammonium chloride was added thereto, and the mixture was extracted three times with ethyl acetate. The combined ethyl acetate layers were washed with water and brine, then dried with anhydrous magnesium sulfate, and subsequently concentrated under vacuum. The obtained crude product was purified by silica gel column chromatography (eluent: hexane/ethyl acetate (v/v)=20/1) to give 570 mg (1.56 mmol equivalents) of 5-benzyloxyethyl-2,2-dimethyl-5-(t-butyldiphenylsiloxymethyl)-1,3-dioxane.

1. customAfter completion of the reaction
2. extractionthe mixture was extracted three times with ethyl acetate
3. washThe combined ethyl acetate layers were washed with water and brine
4. dry with materialdried with anhydrous magnesium sulfate
5. concentrationsubsequently concentrated under vacuum
6. customThe obtained crude product
7. customwas purified by silica gel column chromatography (eluent: hexane/ethyl acetate (v/v)=20/1)