Pyridine → beta-Bromo-beta-nitrostyrene
반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([CH:8](Br)[CH:9]([Br:13])[N+:10]([O-:12])=[O:11])=[CH:4][CH:3]=1.N1C=CC=CC=1>C1CCCCC1>[N+:10]([C:9]([Br:13])=[CH:8][C:5]1[CH:4]=[CH:3][CH:2]=[CH:7][CH:6]=1)([O-:12])=[O:11]참가 물질
4
실험 절차
To a refluxing solution of 1-(4-chlorophenyl)-1,2-dibromo-2-nitroethane (from example 1) in cyclohexane (200 mL) is added a solution of pyridine (6 mL, 74 mmoles) in cyclohexane (200 mL) over a 1 hour period. The mixture is refluxed for an additional hour. The refluxing mixture is then extracted with approximately 200 mL of dilute HCl and 2×200 mL H2O. The organic layer is dried over magnesium sulfate (anhydrous) filtered, and the solvent removed from the filtrate by evaporation to yield a yellow solid. The solid is recrystallized from cyclohexane to give beta-nitrobromostyrene.
후처리
- temperatureThe mixture is refluxed for an additional hour
- extractionThe refluxing mixture is then extracted with approximately 200 mL of dilute HCl and 2×200 mL H2O
- dry with materialThe organic layer is dried over magnesium sulfate (anhydrous)
- filtrationfiltered
- customthe solvent removed from the filtrate by evaporation
- customto yield a yellow solid
- customThe solid is recrystallized from cyclohexane
출처 및 근거
- ORD 기록
- ord-4af8907cc33e4e8a8af3ffab45393966
- 출처 데이터셋
- uspto-grants-1993_01
- 특허 번호
- US05180734
반응 노트
불러오는 중…