반응 #76559

ord-d335b0ed4e1f44deb4d7c29830e9fead

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The reaction mixture was filtered through a layer of Celite®
  2. 2
    여과filter agent
  3. 3
    세척the filter cake was rinsed well with methanol
  4. 4
    workup.ADDITIONThe filtrate was treated with charcoal
  5. 5
    농축concentrated under vacuum
  6. 6
    기타to provide a fluffy pale green solid
  7. 7
    기타This material was triturated with acetonitrile

실험 절차

7-Methyl-3-nitro-4-quinolinol (11.8 g, 58 mmol), methanol (about 300 mL), ammonium hydroxide (50 mL), and palladium on carbon (1 g of 10%) were combined. The mixture was placed on a Parr apparatus under a 35-40 psi (2.4-2.8 Kg/cm2) hydrogen atmosphere for about 1 hour. The reaction mixture was filtered through a layer of Celite® filter agent and the filter cake was rinsed well with methanol. The filtrate was treated with charcoal and then concentrated under vacuum to provide a fluffy pale green solid. This material was triturated with acetonitrile to provide 8.5 g of 3-amino-7-methyl-4-quinolinol.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06703402B2uspto-grants-2004_03