Acetyl chloride → 4'-Chloro-2'-fluoroacetanilide

HRID 52422

反応式

HRID 52422 の反応式
[C:1](Cl)(=[O:3])[CH3:2].[Cl:5][C:6]1[CH:12]=[CH:11][C:9]([NH2:10])=[C:8]([F:13])[CH:7]=1.C(N(CC)CC)C.C(OCC)(=O)C>O1CCCC1.C(O)C>[Cl:5][C:6]1[CH:12]=[CH:11][C:9]([NH:10][C:1](=[O:3])[CH3:2])=[C:8]([F:13])[CH:7]=1

参加物

7

反応物 4

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 938984-Chloro-2-fluoroaniline

生成物 1

HCID 8531744'-Chloro-2'-fluoroacetanilide

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Acetyl chloride (24.2 mL, 0.34 mol) is added slowly to a solution of 4-chloro-2-fluoroaniline (49.4 g, 0.34 mol), and triethylamine (47 mL, 0.34 mol) in tetrahydrofuran while maintaining the reaction mixture temperature below 20° C. After the addition is complete, the reaction mixture is stirred overnight at room temperature, and poured into ethyl acetate. The organic solution is washed sequentially with water and brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to obtain an off-white solid. A mixture of the solid in ethanol is stirred for several minutes, and filtered to give the tilte product as a white solid.

後処理

  1. temperaturewhile maintaining the reaction mixture temperature below 20° C
  2. additionAfter the addition
  3. washThe organic solution is washed sequentially with water and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customto obtain an off-white solid
  7. stirringis stirred for several minutes
  8. filtrationfiltered

出典と根拠

ORDレコード
ord-6a7947b6ec29499281421e7449890a84
出典データセット
uspto-grants-1997_04
特許番号
US05616706

関連ノート

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