Pyridine → beta-Bromo-beta-nitrostyrene
反応式
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]参加物
4
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-92eb4859e3cf452e8687917dfec831e4
- 出典データセット
- uspto-grants-1993_08
- 特許番号
- US05233052
反応ノート
読み込み中…