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

HRID 25306

反応式

HRID 25306 の反応式
[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

参加物

7

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 241Benzene溶媒HCID 8058Hexane溶媒HCID 178418339Butyllithium溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-f2cfb412bf3d4b57a1c11a5247038448
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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