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Bromine → 2,4,5-Trifluorophenacyl bromide

HRID 1711780
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HRID 1711780 반응식
[F:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([F:9])=[CH:4][C:3]=1[C:10](=[O:18])[CH2:11]C1C=CC=CC=1.[Br:19]Br>C(Cl)Cl>[Br:19][CH2:11][C:10]([C:3]1[CH:4]=[C:5]([F:9])[C:6]([F:8])=[CH:7][C:2]=1[F:1])=[O:18]
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참가 물질

4

반응물 2

HCID 24408BromineHCID 685089652',4',5'-Trifluorophenylacetophenone

생성물 1

HCID 27831812,4,5-Trifluorophenacyl bromide수율 98.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A 1 L 3-neck round bottom flask was charged with 2′,4′,5′-trifluorophenylacetophenone (49.7 g, 285 mmol) and DCM (350 mL). The flask was equipped with a 250 mL dropping funnel that contained a solution of bromine (14.6 mL, 283 mmol) in DCM (125 mL). This solution was added to the reaction flask over about 1 h at about 23° C. Once addition of the solution was complete, the reaction mixture was stirred for about 1 h at ambient temperature. Ice water was added to the reaction flask and the mixture was stirred for about 15 min. The layers were separated and the organic solution was then washed with water and brine, dried over MgSO4, filtered, and the solvent was removed under reduced pressure to give the title compound as a pale yellow solid (70.3 g, 97%): LC/MS (Table 1, Method d) Rt=2.20 min; MS m/z 251.0 (M+H)+.

후처리

  1. customThe flask was equipped with a 250 mL
  2. additionThis solution was added to the reaction flask over about 1 h at about 23° C
  3. additionOnce addition of the solution
  4. stirringthe mixture was stirred for about 15 min
  5. customThe layers were separated
  6. washthe organic solution was then washed with water and brine
  7. dry with materialdried over MgSO4
  8. filtrationfiltered
  9. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-9669c747bd984a089f5a57f83b9a0752
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07790741B2

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