Bromine → HCID 178432818、化合物
反応式
[OH:1][C:2]1[C:7]([C:8]([OH:10])=[O:9])=[CH:6][N:5]=[C:4]([CH3:11])[CH:3]=1.[Br:12]Br>C(O)(=O)C.O>[Br:12][C:3]1[C:4]([CH3:11])=[N:5][CH:6]=[C:7]([C:2]=1[OH:1])[C:8]([OH:10])=[O:9]参加物
5
反応条件
- 温度
- 60 °C
実験手順
4-Hydroxy-6-methylnicotinic acid 19 (95.6 g, 0.625 mol) was dissolved in acetic acid (950 ml) and water (190 ml), and bromine (39 ml, 0.750 mol) was added over 15 minutes. After the solution was stirred at 60° C. for 5 hours, the solvent was distilled off under reduced pressure, methanol (200 ml) was added and, crystals were collected by filtration. The solution was distilled off under reduced pressure, methanol was added again to the residue, and crystals were collected by filtration. A total of 142.2 g (98%) of 5-bromo-4-hydroxy-6-methylnicotinic acid 20 was obtained as a colorless crystal.
後処理
- distillationthe solvent was distilled off under reduced pressure, methanol (200 ml)
- additionwas added
- filtrationcrystals were collected by filtration
- distillationThe solution was distilled off under reduced pressure, methanol
- additionwas added again to the residue, and crystals
- filtrationwere collected by filtration
出典と根拠
- ORDレコード
- ord-f43285c516d9484a95a3691547922a55
- 出典データセット
- uspto-grants-2012_05
- 特許番号
- US08188271B2
反応ノート
読み込み中…