HCID 178470035、化合物 → HCID 178516647、化合物
反応式
C(OC(=O)[C:5]1[C:10]([OH:11])=[CH:9][C:8]([C:12]([F:15])([F:14])[F:13])=[N:7][C:6]=1[OH:16])C>Cl>[F:15][C:12]([F:13])([F:14])[C:8]1[N:7]=[C:6]([OH:16])[CH:5]=[C:10]([OH:11])[CH:9]=1参加物
3
反応条件
- 温度
- 100 °C
実験手順
2,4-Dihydroxy-6-trifluoromethyl-nicotinic acid ethyl ester (62 g/247 mmol) was added in several portions over 30 min to 6M HCl(aq) (620 mL) at reflux. Heated at 100° C. overnight with vigorous stirring to obtain complete solution. Allowed to cool and concentrated in vacuo to a white solid. Slurried in water (250 mL) and adjusted to pH 7 with concentrated ammonia to get heavy white suspension. Collected solid by filtration, rinsing through with fresh water, and dried to provide 6-trifluoromethyl-pyridine-2,4-diol (44.0 g) as a white solid.
後処理
- temperatureat reflux
- customto obtain complete solution
- temperatureto cool
- concentrationconcentrated in vacuo to a white solid
- customto get heavy white suspension
- customCollected solid
- filtrationby filtration
- washrinsing through with fresh water
- customdried
出典と根拠
- ORDレコード
- ord-6c6927a6d71946c8831a739cf18d1414
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08372836B2
反応ノート
読み込み中…