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2-Bromo-1-chloro-4-(trifluoromethoxy)benzene → 1-Chloro-2-vinyl-4-(trifluoromethoxy)benzene

HRID 1267894
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HRID 1267894 반응식
Br[C:2]1[CH:7]=[C:6]([O:8][C:9]([F:12])([F:11])[F:10])[CH:5]=[CH:4][C:3]=1[Cl:13].[CH2:14](C([Sn])=C(CCCC)CCCC)[CH2:15]CC>C1(C)C=CC=CC=1>[Cl:13][C:3]1[CH:4]=[CH:5][C:6]([O:8][C:9]([F:12])([F:11])[F:10])=[CH:7][C:2]=1[CH:14]=[CH2:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 27614052-Bromo-1-chloro-4-(trifluoromethoxy)benzeneHCID 53438229Tri(butyl)vinyltin

생성물 1

HCID 185425101-Chloro-2-vinyl-4-(trifluoromethoxy)benzene수율 33.3%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

2-Bromo-1-chloro-4-(trifluoromethoxy)benzene (Description 25; 1.0 g, 3.6 mmol) and tri-n-butylvinyl tin (1.21 g, 3.8 mmol) were dissolved in toluene (20 mL) and the solution was degassed for 45 minutes with nitrogen. Tetrakis(triphenylphosphine) palladium (0) (100 mg) was then added and the solution heated at reflux for 2 hours. Once cooled, the solution was concentrated and the residue was purified by silica chromatography to give the title compound (274 mg, 1.2 mmol).

후처리

  1. customthe solution was degassed for 45 minutes with nitrogen
  2. additionTetrakis(triphenylphosphine) palladium (0) (100 mg) was then added
  3. temperaturethe solution heated
  4. temperatureat reflux for 2 hours
  5. temperatureOnce cooled
  6. concentrationthe solution was concentrated
  7. customthe residue was purified by silica chromatography

출처 및 근거

ORD 기록
ord-42516b6a83aa443da1d965425cf9656c
출처 데이터셋
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06555552B2

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