Diethyl Sulfate → HCID 131729763, compound

Temperature

52 °C

302 grams (0.83 mole) of a ketone mixture of 96.0 percent (CF3)2CFC(O)CF(CF3)2 and 4.0 percent CF3CF2CFC(O)CF(CF3)2, 300 mL anhydrous 1,2-dimethoxyethane, 59.5 grams (1.02 mole) potassium fluoride, 11.1 grams Adogen™ 464 phase transfer catalyst, and 174 grams (1.12 mole) diethyl sulfate were combined in a 2 L flask and heated with stirring to 52° C. for 89 hours. At the end of the 89 hours, the flask was cooled to room temperature, and 230 grams of 45 percent potassium hydroxide and 95 grams of water were added. The resulting mixture was distilled azeotropically using a Dean Stark trap, from which the resulting lower fluorochemical phase was separated during the distillation. The fluorochemical phase was washed twice with an equal volume of water and dried over magnesium sulfate. 53.0 grams of material resulted, with a purity of 37.6 percent (CF3)2CFCF(OC2H5)CF(CF3)2 (yield of 6.1 percent; structure confirmed by GCMS).

1. customwere combined in a 2 L flask
2. temperatureheated
3. temperatureAt the end of the 89 hours, the flask was cooled to room temperature
4. distillationThe resulting mixture was distilled azeotropically
5. customfrom which the resulting lower fluorochemical phase was separated during the distillation
6. washThe fluorochemical phase was washed twice with an equal volume of water
7. dry with materialdried over magnesium sulfate

ORD record

ord-8e6f1323a7564935a3a3b32fa92d8ddd

Source dataset

uspto-grants-2012_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08193397B2