Iodine → 4-Bromo-2-iodo-5-(trifluoromethyl)aniline

HRID 74463

反応式

HRID 74463 の反応式
[I:1]I.[Br:3][C:4]1[CH:10]=[CH:9][C:7]([NH2:8])=[CH:6][C:5]=1[C:11]([F:14])([F:13])[F:12]>S([O-])([O-])(=O)=O.[Ag+2].C(O)C>[Br:3][C:4]1[C:5]([C:11]([F:12])([F:13])[F:14])=[CH:6][C:7]([NH2:8])=[C:9]([I:1])[CH:10]=1

参加物

5

反応物 2

HCID 807IodineHCID 678524-Bromo-3-(trifluoromethyl)aniline

生成物 1

HCID 455880634-Bromo-2-iodo-5-(trifluoromethyl)aniline

試薬・触媒・溶媒 2

HCID 178418844HCID 178418844、化合物触媒HCID 702Ethanol溶媒

実験手順

Iodine (1.4 g, 5.5 mmol, 1.1 eq.) was gradually added to a mixture solution of 4-bromo-3-trifluoromethyl aniline (1.2 g, 1.0 mmol), silver sulfate (1.72 g, 5.5 mmol, 1.1 eq.), and anhydrous ethanol (35 ml). This was stirred at room temperature for two and half hours. The reaction mixture was filtered through Celite, and washed with ethyl acetate. The wash solution was washed with aqueous solutions of 10% sodium thiosulfate, saturated sodium bicarbonate, and saturated sodium chloride, and then dried over anhydrous sodium sulfate. The desiccant was removed by filtration, and concentration was performed. Crude solid 4-bromo-2-iodo-5-trifluoromethyl-phenylamine was obtained by concentration under reduced pressure. The resulting crude product was used in subsequent reactions without being purified.

後処理

  1. filtrationThe reaction mixture was filtered through Celite
  2. washwashed with ethyl acetate
  3. washThe wash solution was washed with aqueous solutions of 10% sodium thiosulfate, saturated sodium bicarbonate, and saturated sodium chloride
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe desiccant was removed by filtration, and concentration

出典と根拠

ORDレコード
ord-d6a33fdfa4b64eaea5e2034d511c5693
出典データセット
uspto-grants-2014_09
特許番号
US08829199B2

関連ノート

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