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Aluminum(III) Chloride → HCID 12574736, 화합물

HRID 1658479
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HRID 1658479 반응식
[Cl:1][C:2]([F:10])([C:6]([Cl:9])([F:8])[F:7])[C:3](F)=[O:4].[Cl-:11].[Al+3].[Cl-].[Cl-]>C(Cl)Cl>[Cl:1][C:2]([F:10])([C:6]([Cl:9])([F:8])[F:7])[C:3]([Cl:11])=[O:4]
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참가 물질

4

반응물 2

HCID 6451240Aluminum(III) ChlorideHCID 133485772,3-Dichloro-2,3,3-trifluoropropanoyl fluoride

생성물 1

HCID 12574736HCID 12574736, 화합물수율 131.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A 100-g sample (0.5 mole) of 2,3-dichloro-2,3,3-trifluoropropionyl fluoride, prepared as shown in Example 11, was added dropwise to a stirred suspension of 34 g (0.25 mole) of aluminum chloride in 200 ml of methylene chloride. The reaction mixture was stirred for two hrs, and the volatile portion was distilled under reduced pressure into a Dry-ice cooled trap. Redistillation gave 70.6 g (66%) of 2,3-dichloro-2,3,3-trifluoropropionyl chloride as a colorless liquid: bp 87.5°-88°; nd 25 1,3812; ir (liquid 5.57μ (C=O); 19F nmr (CCl3F) δ 64.2 ppm (d, J = 173 Hz to d, J = 8 Hz, 1F), 65.7 ppm (d, J = 173 Hz to d, J = Hz, 1F) and 117.4 ppm (d, J = 10 Hz to d, J = 8 Hz, 1F).

후처리

  1. distillationthe volatile portion was distilled under reduced pressure into a Dry-ice cooled trap
  2. distillationRedistillation

출처 및 근거

ORD 기록
ord-ac761de893764d25a7e0c761e2961475
출처 데이터셋
uspto-grants-1976_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03965074

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