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

HRID 70127

반응식

HRID 70127 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-19e6337ddada4661bb84eebb88a950a1
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822472B2

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