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

HRID 1634163
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HRID 1634163 반응식
[F-:1].[K+].CCCCCCCCCC[N+](CCCCCCCCCC)(CCCCCCCCCC)C.CCCCCCCCC[N+](CCCCCCCCC)(CCCCCCCCC)C.CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)C.[Cl-].[Cl-].[Cl-].[C:93]([C:97]([C:99]([C:105]([F:108])([F:107])[F:106])([C:101]([F:104])([F:103])[F:102])[F:100])=O)([F:96])([F:95])[F:94].S([O:114][CH3:115])(OC)(=O)=O.[OH-].[K+]>O.COCCOCCOC>[C:93]([C:97]([C:99]([C:105]([F:108])([F:107])[F:106])([C:101]([F:104])([F:103])[F:102])[F:100])([O:114][CH3:115])[F:1])([F:96])([F:95])[F:94]
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참가 물질

8

반응물 5

HCID 6497Dimethyl SulfateHCID 14797Potassium HydroxideHCID 522689Potassium FluorideHCID 141753771,1,1,3,4,4,4-Heptafluoro-3-(trifluoromethyl)butan-2-oneHCID 16218603Methyl-tri(nonyl)azanium;methyl(trioctyl)azanium;tris-decyl(methyl)azanium;trichloride

생성물 1

HCID 22987398
1,1,1,2,3,4,4,4-Octafluoro-2-methoxy-3-(trifluoromethyl)butane

시약·촉매·용매 2

HCID 962Water용매HCID 8150Diglyme용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-c4e08e1afca24a2cb980500794e6975d
출처 데이터셋
uspto-grants-2003_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06506459B2

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