Bromocyclopropane → Butyl-[1-(2-cyclopropyl-4,6-bis-trifluoromethyl-phenyl)-methylidene]-amine

HRID 39428

反応式

HRID 39428 の反応式
[CH:1]1(Br)[CH2:3][CH2:2]1.[Mg].[CH2:6]([N:10]=[CH:11][C:12]1[C:17]([C:18]([F:21])([F:20])[F:19])=[CH:16][C:15]([C:22]([F:25])([F:24])[F:23])=[CH:14][C:13]=1F)[CH2:7][CH2:8][CH3:9]>C(OCC)C.[Cl-].[Mn+2].[Cl-]>[CH2:6]([N:10]=[CH:11][C:12]1[C:17]([C:18]([F:21])([F:20])[F:19])=[CH:16][C:15]([C:22]([F:25])([F:24])[F:23])=[CH:14][C:13]=1[CH:1]1[CH2:3][CH2:2]1)[CH2:7][CH2:8][CH3:9]

参加物

6

反応物 3

HCID 78037BromocyclopropaneHCID 5462224MagnesiumHCID 58167770Butyl-[1-(2-fluoro-4,6-bis-trifluoromethyl-phenyl)-methylidene]-amine2 回

生成物 1

HCID 58167766Butyl-[1-(2-cyclopropyl-4,6-bis-trifluoromethyl-phenyl)-methylidene]-amine

試薬・触媒・溶媒 2

HCID 10313134Manganese(2+) dichloride触媒HCID 3283Diethyl Ether溶媒

実験手順

Cyclopropylbromide (3.84 g, 32 mmol) was added to magnesium (771 mg, 32 mmol) in 20 mL diethylether and refluxed for 10 min. Manganese(II) chloride (160 mg, 1.27 mmol) and butyl-[1-(2-fluoro-4,6-bis-trifluoromethyl-phenyl)-methylidene]-amine (intermediate M, 4 g, 13 mmol) was added. The reaction mixture was refluxed for 2 h. The reaction mixture was quenched with 8 mL water and filtered through dicalite. The organic phase was separated and dried on sodium sulfate, filtered and evaporated. The crude material, brown oil (3.54 g, 82%) was used without further purification.

後処理

  1. temperaturerefluxed for 10 min
  2. temperatureThe reaction mixture was refluxed for 2 h
  3. customThe reaction mixture was quenched with 8 mL water
  4. filtrationfiltered through dicalite
  5. customThe organic phase was separated
  6. customdried on sodium sulfate
  7. filtrationfiltered
  8. customevaporated
  9. customThe crude material, brown oil (3.54 g, 82%) was used without further purification

出典と根拠

ORDレコード
ord-98c6ae645cf442be9c235d2382fa39de
出典データセット
uspto-grants-2013_09
特許番号
US08524909B2

関連ノート

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