反应详情

A sample of 12 grams (0.05 mols) of 2,2-bis(trifluoromethyl)-4-hydroxymethyl-1,3-dioxolane in 50 ml toluene is treated with 1.93 grams sodium hydride - mineral oil (53.4%, 0.043 mols) at 25°-33° C. The sodium salt is stirred for 2 hours at 35° C. Benzhydryl bromide, 10.6 grams, (0.043 mols) is added at 37° C. and then the temperature is raised to 75°-95° C. for 3 hours. The mixture is filtered and the filtrate washed with water. Vacuum-stripping gives an oil which is dissolved in methanol and clarified by filtration through Super Cel. Yield of product is 17.0 grams at this point. A forerun is distilled in a 4 inch column filled with stainless steel packing, the remainder without packed column. The product obtained is distilled at 137° C. under 0.45 mm of mercury pressure to yield 2,2-bis(trifluoromethyl)-4-diphenylmethoxymethyl-1,3-dioxolane.

1. temperaturethe temperature is raised to 75°-95° C. for 3 hours
2. filtrationThe mixture is filtered
3. washthe filtrate washed with water
4. customVacuum-stripping gives an oil which
5. filtrationclarified by filtration through Super Cel
6. distillationA forerun is distilled in a 4 inch column
7. additionfilled with stainless steel packing
8. customThe product obtained
9. distillationis distilled at 137° C. under 0.45 mm of mercury pressure