반응 #1573

ord-2e03a241be2b4b53bf88ccfacb21967f

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도while maintaining the reaction mixture temperature below 20° C
  2. 2
    workup.ADDITIONAfter the addition
  3. 3
    세척The organic solution is washed sequentially with water and brine
  4. 4
    건조dried over anhydrous magnesium sulfate
  5. 5
    농축concentrated in vacuo
  6. 6
    기타to obtain an off-white solid
  7. 7
    workup.STIRRINGis stirred for several minutes
  8. 8
    여과filtered

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 title product as a white solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05726126uspto-grants-1998_03