2-Fluoroacryloyl chloride → Pentachlorophenyl 2-fluoroprop-2-enoate

HRID 258325

반응식

HRID 258325 반응식
[F:1][C:2](=[CH2:6])[C:3](Cl)=[O:4].[C:7]1([O-:18])[C:12]([Cl:13])=[C:11]([Cl:14])[C:10]([Cl:15])=[C:9]([Cl:16])[C:8]=1[Cl:17].[K+]>C(#N)C>[F:1][C:2](=[CH2:6])[C:3]([O:18][C:7]1[C:8]([Cl:17])=[C:9]([Cl:16])[C:10]([Cl:15])=[C:11]([Cl:14])[C:12]=1[Cl:13])=[O:4]

참가 물질

4

반응물 2

HCID 27833352-Fluoroacryloyl chlorideHCID 23669628Potassium pentachlorophenate

생성물 1

HCID 14008154Pentachlorophenyl 2-fluoroprop-2-enoate수율 51%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

13.9 g (0.128 mol) of α-fluoroacryloyl chloride (obtained in accordance with example 1c) were added dropwise, at a temperature of 25° C., with stirring and in the course of 30 minutes, to a solution of 30 g (0.0985 mol) of potassium pentachlorophenate in 400 ml of anhydrous acetonitrile, and the reaction mixture was then stirred for a further 90 minutes at the same temperature. The solid formed was filtered off and washed with 20 ml of anhydrous acetonitrile. After 0.01 g of hydroquinone monomethyl ether had been added, the volatile constituents in the mixture of filtrate and washing liquor were distilled off and the residue was recrystallized from boiling n-hexane. 17 g (51% of theory) of pentachlorophenyl α-fluoroacrylate were obtained, melting point 90° to 92° C.

후처리

  1. customThe solid formed
  2. filtrationwas filtered off
  3. washwashed with 20 ml of anhydrous acetonitrile
  4. additionAfter 0.01 g of hydroquinone monomethyl ether had been added
  5. additionthe volatile constituents in the mixture of filtrate
  6. washwashing liquor
  7. distillationwere distilled off
  8. customthe residue was recrystallized

출처 및 근거

ORD 기록
ord-17a8ba3607094e28a1520323ac231feb
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05266668

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