3-(Trifluoromethyl)benzoyl chloride → N-(4-iodo-3-methylphenyl)-3-(trifluoromethyl)benzamide

HRID 502697ノート

反応式

HRID 502697 の反応式
[I:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][C:3]=1[CH3:9].CCN(C(C)C)C(C)C.[F:19][C:20]([F:31])([F:30])[C:21]1[CH:22]=[C:23]([CH:27]=[CH:28][CH:29]=1)[C:24](Cl)=[O:25]>C(Cl)Cl>[I:1][C:2]1[CH:8]=[CH:7][C:5]([NH:6][C:24](=[O:25])[C:23]2[CH:27]=[CH:28][CH:29]=[C:21]([C:20]([F:19])([F:30])[F:31])[CH:22]=2)=[CH:4][C:3]=1[CH3:9]

参加物

5

反応物 3

HCID 752573-(Trifluoromethyl)benzoyl chlorideHCID 81531DiisopropylethylamineHCID 27342754-Iodo-3-methylaniline

生成物 1

HCID 68463023N-(4-iodo-3-methylphenyl)-3-(trifluoromethyl)benzamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 4-iodo-3-methyl aniline (200 mg, 0.86 mmol) and iPr2NEt (0.19 mL, 0.95 mmol) in CH2Cl2 (10 mL) was added 3-(trifluoromethyl)benzoyl chloride (0.133 mL, 0.90 mmol). The mixture was allowed to stir at room temperature for 0.5 h at which time it was diluted with CH2Cl2 (20 mL). The organic layer was washed with aq. HCl (10 mL, 1 M), 9% aq. Na2CO3 (10 mL), brine, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The resulting oil was used without further purification.

後処理

  1. washThe organic layer was washed with aq. HCl (10 mL, 1 M), 9% aq. Na2CO3 (10 mL), brine
  2. dry with materialdried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting oil was used without further purification

出典と根拠

ORDレコード
ord-682efe5acc684c7884172e5d2ad5bed8
出典データセット
uspto-grants-2010_08
特許番号
US07776869B2

反応ノート

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