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

HRID 1934355

反応式

HRID 1934355 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-8391c541c77448b0949a4179691ea6e1
出典データセット
uspto-grants-2002_05
特許番号
US06384033B1

関連ノート

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