Triethylamine → N-(3-Bromo-4-methylphenyl)-2-methylpropanamide

HRID 1269138ノート

反応式

HRID 1269138 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][C:8]=1[CH3:9])[NH2:5].C(N(CC)CC)C.[CH3:17][CH:18]([CH3:22])[C:19](Cl)=[O:20]>C1COCC1>[Br:1][C:2]1[CH:3]=[C:4]([NH:5][C:19](=[O:20])[CH:18]([CH3:22])[CH3:17])[CH:6]=[CH:7][C:8]=1[CH3:9]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 62325Isobutyryl chlorideHCID 82187Benzenamine, 3-bromo-4-methyl-

生成物 1

HCID 22048859N-(3-Bromo-4-methylphenyl)-2-methylpropanamide収率 99.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Into a solution of 1.0 g (5.40 mmol) of 3-bromo-4-methylaniline and 0.91 mL (6.50 mmol) of triethylamine in 10 mL THF at 0° C. was slowly added 0.68 mL (6.50 mmol) of 2-methylpropanoyl chloride. The reaction mixture was stirred at room temperature for 2 hours and concentrated in vacuo. The residue was dissolved in CH2Cl2 and washed with H2O, followed by brine. The organic layer was dried over MgSO4 and concentrated in vacuo to give 1.37 g (5.35 mmol, 99%) of the desired product: ESMS m/e: 255.9 (M+H)+.

後処理

  1. customat 0° C.
  2. concentrationconcentrated in vacuo
  3. dissolutionThe residue was dissolved in CH2Cl2
  4. washwashed with H2O
  5. dry with materialThe organic layer was dried over MgSO4
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-1f8b3f0508964c4c920ba3f9131ed0d2
出典データセット
uspto-grants-2007_04
特許番号
US07199135B2

反応ノート

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