Ethanol → 3,3-Diethoxy-2-fluorohex-1-ene

HRID 1154929

반응식

HRID 1154929 반응식
[CH2:1]([C:5]1([O:10][CH2:11][CH3:12])[CH2:7][C:6]1(Cl)[F:8])[CH2:2][CH2:3]C.C(=O)([O-])[O-].[K+].[K+].[CH2:19]([OH:21])[CH3:20]>>[CH2:19]([O:21][C:5]([O:10][CH2:11][CH3:12])([CH2:1][CH2:2][CH3:3])[C:6]([F:8])=[CH2:7])[CH3:20]

참가 물질

4

반응물 3

HCID 702EthanolHCID 11430Potassium CarbonateHCID 127862351-Butyl-2-chloro-1-ethoxy-2-fluorocyclopropane

생성물 1

HCID 127862363,3-Diethoxy-2-fluorohex-1-ene

실험 절차

A stirred solution of 58.4 g. of 2-butyl-1-chloro-2-ethoxy-1-fluorocyclopropane and 166 g. of anhydrous potassium carbonate in 400 ml. of absolute ethanol is heated at reflux for 18 hours. The solution is cooled and the bulk of the ethanol is removed in vacuo. The residue is partitioned with 500 ml. of water and 750 ml. of ether. The ether phase is washed with three 100 ml. portions of brine, dried over potassium carbonate and concentrated in vacuo to provide 54 g. of a pale yellow oil. A 4.45 g. portion of this oil is distilled through a 6 inch Vigreux column having 2.5 g. of the desired product as a colorless liquid, b.p. 80°-81° C., 24 mm.

후처리

  1. temperatureat reflux for 18 hours
  2. temperatureThe solution is cooled
  3. customthe bulk of the ethanol is removed in vacuo
  4. customThe residue is partitioned with 500 ml
  5. washThe ether phase is washed with three 100 ml
  6. dry with materialportions of brine, dried over potassium carbonate
  7. concentrationconcentrated in vacuo
  8. customto provide 54 g
  9. distillationportion of this oil is distilled through a 6 inch Vigreux column

출처 및 근거

ORD 기록
ord-2c5ed16c9eb04798b046b528638d9fac
출처 데이터셋
uspto-grants-1981_11
특허 번호
US04298754

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