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

HRID 1269138

반응식

HRID 1269138 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-1f8b3f0508964c4c920ba3f9131ed0d2
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07199135B2

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