반응 #78479

ord-3b55e0289f314cf88ad1af857b563a3f

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과the mixture was filtered through kieselguhr
  2. 2
    workup.DISTILLATIONthe solvent was distilled off
  3. 3
    기타The filtrate obtained
  4. 4
    기타was evaporated down
  5. 5
    기타the crystalline precipitate was triturated with ether, suction
  6. 6
    여과filtered
  7. 7
    기타dried

실험 절차

3.65 g (12.5 mmol) of 1-methyl-2-[(4-cyanophenyl)oxymethyl]-5-hydroxymethylimidazo[4,5-b]pyridine were dissolved in 500 mL of dichloromethane and mixed with 15.0 g of manganese dioxide. After 96 hours at room temperature, the mixture was filtered through kieselguhr and the solvent was distilled off. The filtrate obtained was evaporated down, the crystalline precipitate was triturated with ether, suction filtered, and dried. Yield: 3.05 g white powder (84% of theory), C16H12N4O2 (292.30); melting point: 231° C.-234° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06710055B2uspto-grants-2004_03