反応 #1573

ord-2e03a241be2b4b53bf88ccfacb21967f

反応方程式

CCOC(C)=O
ethyl acetate
CC(=O)Cl
Acetyl chloride
Nc1ccc(Cl)cc1F
4-chloro-2-fluoroaniline
CCN(CC)CC
triethylamine
CC(=O)Nc1ccc(Cl)cc1F
title product
CC(=O)Nc1ccc(Cl)cc1F
4'--Chloro-2'-fluoroacetanilide

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度while maintaining the reaction mixture temperature below 20° C
  2. 2
    workup.ADDITIONAfter the addition
  3. 3
    洗浄The organic solution is washed sequentially with water and brine
  4. 4
    乾燥dried over anhydrous magnesium sulfate
  5. 5
    濃縮concentrated in vacuo
  6. 6
    その他to obtain an off-white solid
  7. 7
    workup.STIRRINGis stirred for several minutes
  8. 8
    ろ過filtered

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 title product as a white solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05726126uspto-grants-1998_03