Triethylamine → N-(1,1-Dimethylpropyl)-2,4-difluorobenzamide

HRID 1934355

반응식

HRID 1934355 반응식
[C:1]([NH2:6])([CH2:4][CH3:5])([CH3:3])[CH3:2].C(N(CC)CC)C.[F:14][C:15]1[CH:23]=[C:22]([F:24])[CH:21]=[CH:20][C:16]=1[C:17](Cl)=[O:18].C([O-])(O)=O.[Na+]>C(Cl)Cl>[CH3:2][C:1]([NH:6][C:17](=[O:18])[C:16]1[CH:20]=[CH:21][C:22]([F:24])=[CH:23][C:15]=1[F:14])([CH3:3])[CH2:4][CH3:5]

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 689862-Butanamine, 2-methyl-HCID 516892Sodium BicarbonateHCID 5880812,4-Difluorobenzoyl chloride

생성물 1

HCID 9859382N-(1,1-Dimethylpropyl)-2,4-difluorobenzamide수율 103.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of t-amylamine (0.35 ml, 3.0 mmol) and triethylamine (0.56 ml, 4.0 mmol) in methylene chloride (3 ml) was added a solution of 2,4-difluorobenzoyl chloride (0.36 g, 2.0 mmol) in methylene chloride (2 ml) with cooling in an ice-bath, and stirred for 1 hour. The reaction mixture was poured over saturated aqueous NaHCO3 and extracted with ethyl acetate. The extract was washed with saturated aqueous NaHCO3 and dried over MgSO4. The solvent was evaporated to give the title compound (0.47 g; >99%).

후처리

  1. temperaturewith cooling in an ice-bath
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with saturated aqueous NaHCO3
  4. dry with materialdried over MgSO4
  5. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-8391c541c77448b0949a4179691ea6e1
출처 데이터셋
uspto-grants-2002_05
특허 번호
US06384033B1

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