反应详情

温度

20 °C

To a slurry of alcohol of Example 6 (51.3 g, 0.146 moles) in 2-methyltetrahydrofuran (257 ml) was added imidazole (11.9 g, 0.175 moles) and dimethylaminopyridine (1.79 g, 0.015 moles). Chlorotriisopropylsilane (33.9 g, 0.175 moles) was added over 10 minutes and the resultant mixture heated at 50° C. for 18 hours. The reaction was cooled to 20° C. and washed with 1M hydrochloric acid solution (257 ml) and the aqueous extracted with 2-methyltetrahydrofuran (103 ml). The combined organics were washed with 10% w/w sodium chloride solution, then distilled under reduced pressure, and replaced with n-heptane to give a final volume of 513 ml. The resultant slurry was cooled to 5° C. and granulated for 18 hours. The solid was collected by filtration to give the title compound as a white solid (63.0 g, 87%).

1. washwashed with 1M hydrochloric acid solution (257 ml)
2. extractionthe aqueous extracted with 2-methyltetrahydrofuran (103 ml)
3. washThe combined organics were washed with 10% w/w sodium chloride solution
4. distillationdistilled under reduced pressure
5. customto give a final volume of 513 ml
6. temperatureThe resultant slurry was cooled to 5° C.
7. filtrationThe solid was collected by filtration