반응 #605108

ord-c776e78639fe426497427938e228887b

반응 조건

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

후처리

  1. 1
    기타The resulting mixture was flushed with argon
  2. 2
    온도heating
  3. 3
    workup.ADDITIONThe reaction mixture was diluted with water
  4. 4
    추출extracted with ethyl acetate
  5. 5
    건조The organic layer was dried over anhydrous sodium sulphate
  6. 6
    농축concentrated under vacuum
  7. 7
    기타Purification of the crude product by chromatography on silica eluting with 10% EtOAc in hexane

실험 절차

A mixture comprising 7-chloro-2,3-di-p-tolylpyrido[2,3-b]pyrazine (step 1) (2.5 g, 7.24 mmol), ethyl boronic acid (0.748 g, 10.14 mmol) and K2CO3 (2.9 g, 21.73 mmol) was degassed with argon and treated with Pd(PPh3)4(0.418 g, 0.362 mmol). The resulting mixture was flushed with argon and heated at 100° C. for 12 h and heating continued overnight. The reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulphate and concentrated under vacuum. Purification of the crude product by chromatography on silica eluting with 10% EtOAc in hexane afforded the titled compound;

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09115129B2uspto-grants-2015_08