반응 #89370

ord-ca8ed7fd06cf4ff3a8a7b5ac5854dc1b

용매

반응 조건

온도
120°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타was degassed
  2. 2
    기타The solvent was removed in vacuo
  3. 3
    기타to obtain the crude which
  4. 4
    기타was purified by silica gel chromatography (0˜100% DCM/EtOAc)

실험 절차

A mixture of 3-bromo-6-methylpicolinonitrile (1 g, 5.1 mmol), 2-(tributylstannyl)pyridine (2.43 ml, 6.60 mmol), cesium fluoride (150 mg, 10.2 mmol), CuI (193 mg, 1.02 mmol) and Pd(PPh3)4 (586 mg, 0.51 mmol) in DMF (10 mL) was degassed and heated at 120° C. for 1 h in a microwave reactor. The solvent was removed in vacuo to obtain the crude which was purified by silica gel chromatography (0˜100% DCM/EtOAc) to yield the title compound as a brown oil (0.87 g, 88%). MS (ESI) 196 (M+H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09440982B2uspto-grants-2016_09