반응 #213964
ord-d0be66b2fc944091853bf40e48a5cbc6
용매
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도the resulting solution refluxed for 162 hours
- 2온도The reaction mixture was cooled
- 3농축concentrated
- 4workup.ADDITIONUpon pouring the
- 5농축concentrate into approximately 300 ml of water
- 6기타an off-white solid precipitated which
- 7여과was collected by filtration
- 8기타Recrystallization 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.