Dimethyl Sulfate → 1,1,1,2,3,4,4,4-Octafluoro-2-methoxy-3-(trifluoromethyl)butane

The title compound was prepared essentially as in Example 3 using anhydrous potassium fluoride (12.8 g, 0.22 mol), anhydrous diethylene glycol dimethyl ether (diglyme, 106 g), methyltrialkyl(C8-C10)ammonium chloride (Adogen™ 464, available from Aldrich Chemical Company, 4 g), CF3COCF(CF3)2 (53.2 g, 0.20 mol, prepared essentially by the procedure of Smith et al., J. Am. Chem. Soc., 84, 4285 (1962)), and dimethyl sulfate (33.9 g, 0.72 mol). Aqueous potassium hydroxide was added to the reaction mixture (approximately 25 g of 50% solution), followed by water (200 mL). The resulting crude product was azeotropically distilled from the reaction mixture. The lower phase of the resulting distillate was separated from the upper phase, was washed with water, was dried over anhydrous sodium sulfate, and was distilled (b.p. 82-83° C.; yield of 45 g). The product identity was confirmed by GCMS and by FTIR.

1. customprepared essentially by the procedure of Smith et al., J
2. distillationThe resulting crude product was azeotropically distilled from the reaction mixture
3. customThe lower phase of the resulting distillate was separated from the upper phase
4. washwas washed with water
5. dry with materialwas dried over anhydrous sodium sulfate
6. distillationwas distilled (b.p. 82-83° C.; yield of 45 g)

ORDレコード

ord-2ef118ef9c1841109c70084279b30001

出典データセット

uspto-grants-2003_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06548471B2