Calcium Chloride → HCID 178507679、化合物

HRID 1026547ノート

反応式

HRID 1026547 の反応式
[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

参加物

5

反応物 2

HCID 5284359Calcium ChlorideHCID 178526657HCID 178526657、化合物

生成物 1

HCID 178507679HCID 178507679、化合物収率 71.3%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-3d84b51c89c04dcdb4b987d199d70681
出典データセット
uspto-grants-2014_05
特許番号
US08729095B2

反応ノート

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