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Acetylene → HCID 53816865, 화합물

HRID 1199753
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HRID 1199753 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

HCID 53816865HCID 53816865, 화합물

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4c82c369844a419aa7609e0b592d25f5
출처 데이터셋
uspto-grants-1990_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04902795

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