Water → 4-(2,6-Dichloro-4-trifluoromethylphenyl)toluene

HRID 25300

반응식

HRID 25300 반응식
I[C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][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.C(OCC)C>[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]=1[C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][CH:3]=1

참가 물질

8

반응물 3

HCID 962WaterHCID 122074-IodotolueneHCID 157026Benzene, 1,3-dichloro-2-fluoro-5-(trifluoromethyl)-

생성물 1

HCID 221709614-(2,6-Dichloro-4-trifluoromethylphenyl)toluene수율 85.1%

시약·촉매·용매 4

HCID 241Benzene용매HCID 3283Diethyl Ether용매HCID 8058Hexane용매HCID 178418339Butyllithium용매

실험 절차

To 5.7 g (26.1 mmol) of 4-iodotoluene in 30 ml of dry benzene, 17.0 ml of a n-butyllithium solution in hexane (1.60 mol/l) was added dropwise in a nitrogen stream at room temperature with stirring. After 2 hours of stirring at room temperature, 10 ml of 6.0 g (25.8 mmol) of 3,5-dichloro-4-fluorobenzotrifluoride in 10 ml of diethyl ether was added dropwise at 10° C. After another 12 hours of stirring at room temperature, the reaction mixture was poured into 100 ml of water for separation. The organic layer was washed with 50 ml of water twice and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 6.7 g of 4-(2,6-dichloro-4-trifluoromethylphenyl)toluene (yield 85.0%) as a colorless liquid.

후처리

  1. stirringAfter 2 hours of stirring at room temperature
  2. stirringAfter another 12 hours of stirring at room temperature
  3. washThe organic layer was washed with 50 ml of water twice
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-f6684658b36d49068df1c594071a36ff
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06858639B2

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