반응 #71492

ord-bb9893d1517843b889e27ea5cea8b4a7

용매

반응 조건

온도
150°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타was obtained),
  2. 2
    온도to cool to rt
  3. 3
    추출extracted with Et2O
  4. 4
    workup.ADDITIONThe aqueous phase was acidified to pH 5 by addition of HCl
  5. 5
    여과Vacuum filtration of the resulting suspension

실험 절차

KOH (6.0 g, 107 mmol, 10 equiv) was added to 8-(3,5-dimethoxy-phenyl)-quinoxaline-5-carbonitrile (Step 179.3) (3.12 g, 10.7 mmol) in ethylene glycol (30 mL). The reaction mixture was stirred at 150° C. for 3 h (a solution was obtained), allowed to cool to rt, diluted with Et2O/H2O, and extracted with Et2O. The aqueous phase was acidified to pH 5 by addition of HCl. Vacuum filtration of the resulting suspension afforded 3.3 g of the title compound as a yellow solid: ESI-MS: 311 [M+H]+; tR=4.34 min (System 1).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08536175B2uspto-grants-2013_09