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

HRID 25300

反応式

HRID 25300 の反応式
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

参加物

8

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 4

HCID 241Benzene溶媒HCID 3283Diethyl Ether溶媒HCID 8058Hexane溶媒HCID 178418339Butyllithium溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f6684658b36d49068df1c594071a36ff
出典データセット
uspto-grants-2005_02
特許番号
US06858639B2

関連ノート

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