Water → Benzene, 1,1'-oxybis[4-methyl-

HRID 262432

반응식

HRID 262432 반응식
F[C:2](F)=[C:3](F)F.[K].[CH:8]1[C:13]([OH:14])=[CH:12][CH:11]=[C:10]([CH3:15])[CH:9]=1.O>CN(C)C=O>[C:13]1([O:14][C:8]2[CH:13]=[CH:12][C:2]([CH3:3])=[CH:10][CH:9]=2)[CH:12]=[CH:11][C:10]([CH3:15])=[CH:9][CH:8]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 2879P-CresolHCID 8301TetrafluoroethyleneHCID 5462222Potassium

생성물 1

HCID 74098Benzene, 1,1'-oxybis[4-methyl-

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

Tetrafluoroethylene pentamer (50 g) was added dropwise to the potassium salt of p-cresol (15 g) stirred in dry dimethyl formamide (100 ml) at 30° C. After addition of the pentamer, the reaction mixture was stirred for 45 minutes at 60° C. The cooled reaction mixture was poured into water. The oil which separated out was dissolved in ether, the ether layer washed with water, dried over magnesium sulphate, and distilled to give 40 g of the p-cresyl ether, C10F19OC6H4CH3, boiling point 110° C. to 114° C. at 10 mm Hg. Elementary analysis, infra-red spectra, mass spectrometry and nuclear magnetic resonance measurements confirmed the identity of the compound.

후처리

  1. additionAfter addition of the pentamer
  2. customThe cooled reaction mixture
  3. customThe oil which separated out
  4. dissolutionwas dissolved in ether
  5. washthe ether layer washed with water
  6. dry with materialdried over magnesium sulphate
  7. distillationdistilled

출처 및 근거

ORD 기록
ord-93f1cc33df1c455eb6b768d16eca89f3
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04154753

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