반응 #213964

ord-d0be66b2fc944091853bf40e48a5cbc6

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the resulting solution refluxed for 162 hours
  2. 2
    온도The reaction mixture was cooled
  3. 3
    농축concentrated
  4. 4
    workup.ADDITIONUpon pouring the
  5. 5
    농축concentrate into approximately 300 ml of water
  6. 6
    기타an off-white solid precipitated which
  7. 7
    여과was collected by filtration
  8. 8
    기타Recrystallization from absolute ethanol

실험 절차

In a 250-ml single-necked, round-bottomed flask containing a solution of 3.0 g (75 mmol) of sodium hydroxide in 100 ml of absolute ethanol was added 9.28 g (67 mmol) of 3-nitrophenol at which point the solution turned dark red. To the dark red solution, 10.0 g (66 mmol) of 2,3-dichloropyrazine was added and the resulting solution refluxed for 162 hours. The reaction mixture was cooled and concentrated. Upon pouring the concentrate into approximately 300 ml of water, an off-white solid precipitated which was collected by filtration. Recrystallization from absolute ethanol gave the product, 2-chloro-3-(3-nitrophenoxy)pyrazine, (46% yield) as white needles, mp 119°-121° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04254125uspto-grants-1981_03