반응 #726234

ord-cdac4f8bfadb4d43b5e32cb834e0c950

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGThe reaction was stirred at 0° C. for 30 min
  2. 2
    기타was quenched with glacial AcOH (2.5 mL)
  3. 3
    기타The solvent was removed in vacuo

실험 절차

3-Hydroxy-2-nitropyridine (20 g, 0.143 mole) was dissolved in methanol (400 mL) and a solution of 25% sodium methoxide in methanol (33 mL, 0.13 mole) was added at room temperature. The mixture was stirred for 30 min, then was cooled to 0° C., and bromine (7.2 mL, 0.14 mole) was added slowly. The reaction was stirred at 0° C. for 30 min, then was quenched with glacial AcOH (2.5 mL). The solvent was removed in vacuo to afford material (30 g, 96%), which was used without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07691850B2uspto-grants-2010_04