تفاعل #1573

ord-2e03a241be2b4b53bf88ccfacb21967f

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwhile maintaining the reaction mixture temperature below 20° C
  2. 2
    workup.ADDITIONAfter the addition
  3. 3
    غسيلThe organic solution is washed sequentially with water and brine
  4. 4
    تجفيفdried over anhydrous magnesium sulfate
  5. 5
    تركيزconcentrated in vacuo
  6. 6
    أخرىto obtain an off-white solid
  7. 7
    workup.STIRRINGis stirred for several minutes
  8. 8
    ترشيحfiltered

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05726126uspto-grants-1998_03