반응 #6276

ord-32b0f994e35548499b85f980112ef12f

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 chloroform/ether

실험 절차

Under nitrogen atmosphere, to a solution of 452 mg (1.5 mmol) of 2-[4-(2-aminobenzoylamino)butylthio]pyridine in 20 ml of tetrahydrofuran, 486 mg (3.0 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 chloroform/ether to give 337 mg of the desired product (68.8% yield, white crystals).

출처

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