반응 #979146

ord-4d0b2680644e47faabe84f4839a8f0e0

용매

반응 조건

온도
65°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction mixture is cooled to ambient temperature
  2. 2
    기타the solvents are evaporated under reduced pressure
  3. 3
    workup.ADDITIONThe residue is diluted with 700 uL of DMSO
  4. 4
    여과filtered
  5. 5
    기타purified with preparative reverse phase chromatography

실험 절차

4-Aminonicotinaldehyde (100 mg, 0.78 millimole (hereinafter “mmol”)), 2,6-dichlorophenylacetonitrile (217 mg, 1.2 mmol), 10% aqueous NaOH (0.101 mL, 0.25 mmol) and 700 uL of absolute ethanol are combined and heated at 65° C. for 24 hours (hereinafter “h”). The reaction mixture is cooled to ambient temperature and the solvents are evaporated under reduced pressure. The residue is diluted with 700 uL of DMSO filtered and purified with preparative reverse phase chromatography to afford the title compound as a yellow solid (191 mg, 84% yield). MS ES+ m/z=290.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07005434B2uspto-grants-2006_02