Carbon Disulfide → (1,3)Oxazolo(4,5-b)pyridine-2-thiol
反応式
[OH:1][C:2]1[C:3]([NH2:8])=[N:4][CH:5]=[CH:6][CH:7]=1.[OH-].[K+].[C:11](=S)=[S:12]>CCO>[O:1]1[C:2]2[C:3](=[N:4][CH:5]=[CH:6][CH:7]=2)[NH:8][C:11]1=[S:12]参加物
5
実験手順
3-Hydroxy-2-aminopyridine (2.00 g, 18.2 mmol) and potassium hydroxide (1.22 g, 21.8 mmol) were dissolved in carbon disulfide (15 mL) and EtOH (25 mL), and the reaction mixture was heated to reflux overnight. Upon cooling to rt, the reaction mixture was concentrated under reduced pressure. The resulting solid was suspended in 1 M aqueous HCl, collected by filtration, washed with water (2×) and air-dried. Further drying in a 35° C. vacuum oven gave 2.52 g (91%) of the title compound as a tan solid. LC-MS: RT=4.82 min., [M+H]+=153.1
後処理
- temperatureto reflux overnight
- concentrationthe reaction mixture was concentrated under reduced pressure
- filtrationcollected by filtration
- washwashed with water (2×)
- customair-dried
- customFurther drying in a 35° C. vacuum oven
出典と根拠
- ORDレコード
- ord-19e6337ddada4661bb84eebb88a950a1
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08822472B2
反応ノート
読み込み中…