Triethylamine → N-(5-bromo-2,4-difluorophenyl)-2-methylpropanamide

HRID 1269174노트

반응식

HRID 1269174 반응식
[Br:1][C:2]1[C:3]([F:10])=[CH:4][C:5]([F:9])=[C:6]([CH:8]=1)[NH2:7].C(N(CC)CC)C.[C:18](Cl)(=[O:22])[CH:19]([CH3:21])[CH3:20]>C1COCC1>[Br:1][C:2]1[C:3]([F:10])=[CH:4][C:5]([F:9])=[C:6]([NH:7][C:18](=[O:22])[CH:19]([CH3:21])[CH3:20])[CH:8]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 62325Isobutyryl chlorideHCID 27832955-Bromo-2,4-difluoroaniline

생성물 1

HCID 16757161N-(5-bromo-2,4-difluorophenyl)-2-methylpropanamide수율 94%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Into a solution of 2.6 g (12.6 mmol) of 5-bromo-2,4-difluoroaniline and 2.1 mL (15.1 mmol) of triethylamine in 50 mL THF at 0° C. was slowly added 1.6 mL (15.1 mmol) of isobutyryl chloride. The reaction mixture was stirred at room temperature for 2 hours and concentrated in vacuo. The residue was dissolved in EtOAc and washed with H2O, saturated aqueous Na2CO3 and brine. The organic layer was dried over MgSO4 and concentrated in vacuo to give 3.3 g (11.8 mmol, 94%) of N-(5-bromo-2,4-difluorophenyl)-2-methylpropanamide: ESMS m/e: 278.1 (M+H)+.

후처리

  1. customat 0° C.
  2. concentrationconcentrated in vacuo
  3. dissolutionThe residue was dissolved in EtOAc
  4. washwashed with H2O, saturated aqueous Na2CO3 and brine
  5. dry with materialThe organic layer was dried over MgSO4
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-cd842e07ce064aa2af7191fd639a8802
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07199135B2

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