Phosphorus oxybromide → 2-Bromo-5-methyl-3-nitropyridine
反応式
P(Br)(Br)([Br:3])=O.O[C:7]1[C:12]([N+:13]([O-:15])=[O:14])=[CH:11][C:10]([CH3:16])=[CH:9][N:8]=1>CN(C=O)C>[Br:3][C:7]1[C:12]([N+:13]([O-:15])=[O:14])=[CH:11][C:10]([CH3:16])=[CH:9][N:8]=1参加物
4
反応条件
- 温度
- 5 °C
実験手順
POBr3 (222.8 g, 0.78 mol) was added in portions to 2-hydroxy-5-methyl-3-nitropyridine (100 g, 0.65 mol) in DMF (500 mL) with stirring at 0-10° C. then the reaction mixture was stirred at 80° C. under nitrogen for 12 hours. Reaction mixture was cooled and poured into crushed ice (1 Kg), obtained solid was filtered, washed thoroughly with ice-cold water (2×500 mL), dried in a desiccator under high vacuum for one day to obtain 2-bromo-5-methyl-3-nitropyridine as yellow solid (121 g) in 86% yield. (M+H) Expected: 217; found 216.9.
後処理
- stirringthe reaction mixture was stirred at 80° C. under nitrogen for 12 hours
- customReaction mixture
- temperaturewas cooled
- additionpoured
- customobtained solid
- filtrationwas filtered
- washwashed thoroughly with ice-cold water (2×500 mL)
- customdried in a desiccator under high vacuum for one day
出典と根拠
- ORDレコード
- ord-811edca51b1a421ea6eee0f08a6ef749
- 出典データセット
- uspto-grants-2013_10
- 特許番号
- US08546408B2
反応ノート
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