Dimethyl Sulfate → Methyl perfluoroisobutyl ether
Reaction equation
[F-:1].[K+].[F:3][C:4]([C:12]([F:15])([F:14])[F:13])([C:8]([F:11])([F:10])[F:9])[C:5]([F:7])=O.S([O:21][CH3:22])(OC)(=O)=O>CN(C)C=O>[C:4]([C:5]([O:21][CH3:22])([F:1])[F:7])([C:12]([F:15])([F:14])[F:13])([C:8]([F:11])([F:10])[F:9])[F:3]Participants
5
Conditions
- Temperature
- 40 °C
Procedure
The title compound was prepared essentially as in Example 1 using anhydrous potassium fluoride (31.9 g, 0.55 mole), anhydrous dimethyl formamide (186 g), perfluoroisobutryl fluoride (108 g of 99% purity, 0.5 mole), and dimethyl sulfate (81.9 g, 0.65 mole). The resulting mixture was held at −20° C. for 16 hours, was warmed to 40° C. for 3.5 hours, and was then distilled to yield 109 g of the title compound (83.6% purity by GLC; also containing 11.6% (CF3)2CFCOF). The reaction mixtures from several runs were combined and distilled (b.=60-61° C.).
Workup
- distillationwas then distilled
Sources & evidence
- ORD record
- ord-8183a13b370d4c73aa697b285b8a3b1d
- Source dataset
- uspto-grants-2003_01
- Patent number
- US06509309B2
Reaction notes
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