Water → 1-Chloro-3-(2,6-dichloro-4-trifluoromethylphenyl)benzene

HRID 25306

반응식

HRID 25306 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4](I)[CH:3]=1.[Cl:9][C:10]1[CH:11]=[C:12]([C:18]([F:21])([F:20])[F:19])[CH:13]=[C:14]([Cl:17])[C:15]=1F.O>C1C=CC=CC=1.C([Li])CCC.CCCCCC>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([C:15]2[C:14]([Cl:17])=[CH:13][C:12]([C:18]([F:19])([F:21])[F:20])=[CH:11][C:10]=2[Cl:9])[CH:3]=1

참가 물질

7

반응물 3

HCID 962WaterHCID 122691-Chloro-3-iodobenzeneHCID 157026Benzene, 1,3-dichloro-2-fluoro-5-(trifluoromethyl)-

생성물 1

HCID 221709261-Chloro-3-(2,6-dichloro-4-trifluoromethylphenyl)benzene수율 36.7%

시약·촉매·용매 3

HCID 241Benzene용매HCID 8058Hexane용매HCID 178418339Butyllithium용매

실험 절차

To 10.0 g (41.9 mmol) of 1-chloro-3-iodobenzene in 50 ml of dry benzene, 32.0 ml of a n-butyllithium solution in hexane (1.56 mol/l) was added dropwise in a nitrogen stream at room temperature with stirring. After another 2 hours of stirring at room temperature, 9.9 g (42.5 mmol) of 3,5-dichloro-4-fluorobenzotrifluoride was added dropwise at 10° C. After another 12 hours of stirring at room temperature, the reaction mixture was poured into 500 ml of water for separation. The organic layer was washed with 200 ml of water twice and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. Purification of the residue by silica gel column chromatography afforded 5.0 g of 1-chloro-3-(2,6-dichloro-4-trifluoromethylphenyl)benzene (yield 35.0%).

후처리

  1. stirringAfter another 2 hours of stirring at room temperature
  2. stirringAfter another 12 hours of stirring at room temperature
  3. washThe organic layer was washed with 200 ml of water twice
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customPurification of the residue by silica gel column chromatography

출처 및 근거

ORD 기록
ord-f2cfb412bf3d4b57a1c11a5247038448
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06858639B2

연결된 노트

불러오는 중…