反应详情

温度

-20 °C

A jacketed one liter round bottom flask was equipped with an overhead stirrer, a solid carbon dioxide/acetone condenser, and an addition funnel. The flask was charged with spray-dried potassium fluoride (85 g, 1.46 mol) and anhydrous diethylene glycol dimethyl ether (375 g) and was then cooled to about −20° C. using a recirculating refrigeration system. C2F5COF (196 g, 1.18 mol) was added to the flask over a period of about one hour. The flask was then warmed to about 24° C., and dimethyl sulfate (184.3 g, 1.46 mol) was then added dropwise via the addition funnel over a 45 minute period. The resulting mixture was then stirred at room temperature overnight. Water (a total of 318 mL) was then added dropwise to the mixture. The mixture was transferred to a one liter round bottom flask, and the resulting product ether was azeotropically distilled. The lower product phase of the resulting distillate was separated from the upper aqueous phase, was washed once with cold water, and was subsequently distilled to give 180 g of product (b.p. 36° C.;>99.9% purity by GLC). The product identity was confirmed by GCMS and by 1H and 19F NMR.

1. customA jacketed one liter round bottom flask was equipped with an overhead stirrer, a solid carbon dioxide/acetone condenser, and an addition funnel
2. temperatureThe flask was then warmed to about 24° C.
3. customThe mixture was transferred to a one liter round bottom flask
4. distillationthe resulting product ether was azeotropically distilled
5. customThe lower product phase of the resulting distillate was separated from the upper aqueous phase
6. washwas washed once with cold water
7. distillationwas subsequently distilled