반응 #3963

ord-9bb33ecc109041f0a8377bc723501737

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The mixture is filtered off from the catalyst
  2. 2
    workup.ADDITIONthe mother liquor is mixed with 100 ml each of ether and of ethyl acetate, and finally 3 ml of etheral hydrochloric acid
  3. 3
    workup.ADDITIONare added
  4. 4
    기타The precipitate is recrystallized from methanol
  5. 5
    건조After drying over phosphorus pentoxide and potassium hydroxide
  6. 6
    기타a product is obtained which

실험 절차

An amount of 1.7 gm of 2-(2-dimethylamino-4-nitro-phenyl)-4H-imidazo[4,5-b]pyridin-5-one is dissolved in 20 ml of dimethylformamide and mixed with 0.2 gm of 10% palladium/charcoal. The mixture is hydrogenated for three hours with hydrogen at ambient temperature under 5 bars of pressure. The mixture is filtered off from the catalyst, the mother liquor is mixed with 100 ml each of ether and of ethyl acetate, and finally 3 ml of etheral hydrochloric acid are added. The precipitate is recrystallized from methanol. After drying over phosphorus pentoxide and potassium hydroxide, a product is obtained which contains 1.5 mol of hydrochloric acid and 0.5 mol of water to 1 mol of base.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04722929uspto-grants-1988_02