Calcium Chloride → HCID 178507679, 화합물

HRID 1026547노트

반응식

HRID 1026547 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([N+:9]([O-])=O)[C:5]([OH:8])=[N:6][CH:7]=1.[Cl-].[Ca+2].[Cl-]>[Fe].C(O)C>[NH2:9][C:4]1[C:5]([OH:8])=[N:6][CH:7]=[C:2]([Cl:1])[CH:3]=1

참가 물질

5

반응물 2

HCID 5284359Calcium ChlorideHCID 178526657HCID 178526657, 화합물

생성물 1

HCID 178507679HCID 178507679, 화합물수율 71.3%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 702Ethanol용매

실험 절차

To an 80% aqueous ethanol suspension (150 ml) of 5-chloro-3-nitropyridin-2-ol (15.0 g) and calcium chloride (9.54 g) was added iron powder (24.0 g), followed by stirring at room temperature for 30 minutes, and further under heating at reflux for 1 hour. After the temperature was brought back to room temperature, the reaction suspension was filtered through Celite. Water was added to the filtrate, and extracted 8 times with a methanol-dichloromethane (1:10) mixed solvent. The collected organic layer was dried over anhydrous sodium sulfate, and concentrated under reduced pressure to afford 3-amino-5-chloropyridin-2-ol (8.86 g).

후처리

  1. temperaturefurther under heating
  2. temperatureat reflux for 1 hour
  3. customwas brought back to room temperature
  4. filtrationthe reaction suspension was filtered through Celite
  5. additionWater was added to the filtrate
  6. extractionextracted 8 times with a methanol-dichloromethane (1:10)
  7. additionmixed solvent
  8. dry with materialThe collected organic layer was dried over anhydrous sodium sulfate
  9. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-3d84b51c89c04dcdb4b987d199d70681
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08729095B2

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