Carbon Disulfide → (1,3)Oxazolo(4,5-b)pyridine-2-thiol

HRID 1487703

反応式

HRID 1487703 の反応式
[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

反応物 3

HCID 6348Carbon DisulfideHCID 14797Potassium HydroxideHCID 281142-Amino-3-Hydroxypyridine

生成物 1

HCID 658727(1,3)Oxazolo(4,5-b)pyridine-2-thiol収率 91%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

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

  1. temperatureto reflux overnight
  2. concentrationthe reaction mixture was concentrated under reduced pressure
  3. filtrationcollected by filtration
  4. washwashed with water (2×)
  5. customair-dried
  6. customFurther drying in a 35° C. vacuum oven

出典と根拠

ORDレコード
ord-871eaabfd49c43c689f266cf4b065d7b
出典データセット
uspto-grants-2016_08
特許番号
US09428522B2

関連ノート

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