반응 #604860

ord-29dd7edd4ae446d6a6fd40fa78731d2d

반응 조건

온도
100°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooled to rt
  2. 2
    추출extracted with EtOAc (2×)
  3. 3
    건조The combined organics were dried (Na2SO4)
  4. 4
    농축concentrated
  5. 5
    기타Purification via silica gel chromatography (5-60% EtOAc in hexanes)

실험 절차

To 2-bromo-6-methyl-3-(2H-1,2,3-triazol-2-yl)pyridine (1.5 g, 7.6 mmol) in DMF (19 mL) was added K2CO3 (1.2 g, 8.4 mmol) and 2H-1,2,3-triazole (440 μL, 7.6 mmol). The mixture was heated to 100° C. for 16 h, cooled to rt and extracted with EtOAc (2×). The combined organics were dried (Na2SO4) and concentrated. Purification via silica gel chromatography (5-60% EtOAc in hexanes) gave the title compound (490 mg, 35%) and 5-methyl-3-(1H-1,2,3-triazol-1-yl)picolinonitrile (387 mg, 27%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09115117B2uspto-grants-2015_08