Dimethyl Carbonate → Methyl Pentafluoroethanesulfonate

반응식

[F:1][C:2]([F:21])([F:20])[C:3]([F:19])([F:18])[S:4]([O:7]S(C(F)(F)C(F)(F)F)(=O)=O)(=[O:6])=[O:5].F[C:23](F)(F)C(F)(F)S(O)(=O)=O.C(=O)(OC)OC>>[F:1][C:2]([F:21])([F:20])[C:3]([F:19])([F:18])[S:4]([O:7][CH3:23])(=[O:6])=[O:5]

참가 물질

반응물 3

HCID 12021Dimethyl Carbonate

HCID 10219841Pentafluoroethanesulfonic acid

HCID 12694826Pentafluoroethanesulfonic anhydride

생성물 1

HCID 22020310Methyl Pentafluoroethanesulfonate수율 84.1%

실험 절차

5.74 g (15.0 mmol) of pentafluoroethanesulfonic anhydride and 0.31 g (1.55 mmol) of pentafluoroethanesulfonic acid are initially introduced in a 10 ml round-necked flask. 1.35 g (15.0 mmol) of dimethyl carbonate are added at room temperature with constant stirring and reflux cooling. The solution is stirred for one hour at a temperature of 60° C. and subsequently for a further 3 hours at 110° C. After distillation, 5.41 g of methyl pentafluoroethanesulfonate are isolated (boiling range: 114–115° C., yield: 84.1%).

후처리

temperaturereflux
temperaturecooling
stirringThe solution is stirred for one hour at a temperature of 60° C. and subsequently for a further 3 hours at 110° C
distillationAfter distillation, 5.41 g of methyl pentafluoroethanesulfonate
customare isolated (boiling range: 114–115° C., yield: 84.1%)

출처 및 근거

ORD 기록: ord-8b47c9918eef431b95489edd655f8465
출처 데이터셋: uspto-grants-2006_08
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US07084290B2

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