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

HRID 52422

반응식

HRID 52422 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

HCID 8531744'-Chloro-2'-fluoroacetanilide

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6a7947b6ec29499281421e7449890a84
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616706

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