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

HRID 1154929

反応式

HRID 1154929 の反応式
[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]

参加物

4

反応物 3

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

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2c5ed16c9eb04798b046b528638d9fac
出典データセット
uspto-grants-1981_11
特許番号
US04298754

関連ノート

読み込み中…