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Acetylene → HCID 53816865、化合物

HRID 1199753
ノート
印刷プレビュー

反応式

HRID 1199753 の反応式
[F:1][C:2]1[C:10]([F:11])=[C:9]([F:12])[C:8]([F:13])=[CH:7][C:3]=1[C:4](Cl)=[O:5].[Cl-:14].[Al+3].[Cl-].[Cl-].[CH:18]#[CH:19]>ClCCCl>[Cl:14][CH:18]=[CH:19][C:4]([C:3]1[CH:7]=[C:8]([F:13])[C:9]([F:12])=[C:10]([F:11])[C:2]=1[F:1])=[O:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6326AcetyleneHCID 27336892,3,4,5-Tetrafluorobenzoyl chlorideHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 53816865HCID 53816865、化合物

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

53.2 g of 2,3,4,5-tetrafluorobenzoyl chloride are added dropwise to a suspension of 36.5 g of anhydrous aluminum chloride in 100 ml of 1,2-dichloroethane at 0°-10° C., while cooling with ice and stirring. Acetylene is then passed in at 40°-50° C. for 7 hours and the mixture is poured onto ice. The phases are separated, subsequent extraction with methylene chloride is carried out and the extract is washed with water and dried with sodium sulphate. The solvent is distilled off in vacuo and the residue is distilled under a high vacuum. 49.2 g of 2,3,4,5-tetrafluorophenyl 2-chlorovinyl ketone pass over at 92°-105° C./1.5 mbar.

後処理

  1. temperaturewhile cooling with ice
  2. additionthe mixture is poured onto ice
  3. customThe phases are separated
  4. extractionsubsequent extraction with methylene chloride
  5. washthe extract is washed with water
  6. dry with materialdried with sodium sulphate
  7. distillationThe solvent is distilled off in vacuo
  8. distillationthe residue is distilled under a high vacuum
  9. customover at 92°-105° C./1.5 mbar

出典と根拠

ORDレコード
ord-4c82c369844a419aa7609e0b592d25f5
出典データセット
uspto-grants-1990_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04902795

反応ノート

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