반응 #6274

ord-ec2bad3e6dba47c4a66e47e6b4dbd056

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.DISTILLATIONThe solvent was distilled off
  2. 2
    workup.DISSOLUTIONthe residue was dissolved in chloroform
  3. 3
    세척The solution was washed with water
  4. 4
    기타dried
  5. 5
    workup.DISTILLATIONThe solvent was distilled off
  6. 6
    기타the residue was recrystallized from ethanol/chloroform/ether

실험 절차

Under nitrogen atmosphere, to a solution of 718 mg (2.5 mmol) of 4-[3-(2-aminobenzoylamino)propylthio]pyridine in 15 ml of tetrahydrofuran. 811 mg (5.0 mmol) of 1,1'carbonyldiimidazole was added, and the mixture was stirred at room temperature for 16 hours. The solvent was distilled off and the residue was dissolved in chloroform. The solution was washed with water and dried. The solvent was distilled off and the residue was recrystallized from ethanol/chloroform/ether to give 514 mg of the desired product (65.7% yield, white crystals).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05246948uspto-grants-1993_09