Hydrazine Sulfate → HCID 88768920、化合物

HRID 629201ノート

反応式

HRID 629201 の反応式
[Cl:1][C:2]1[C:7]2[C:8](=O)[O:9][CH:10](O)[C:6]=2[CH:5]=[C:4]([Cl:13])[N:3]=1.S(O)(O)(=O)=O.[NH2:19][NH2:20].C([O-])(=O)C.[Na+]>O>[Cl:1][C:2]1[C:7]2[C:8](=[O:9])[NH:19][N:20]=[CH:10][C:6]=2[CH:5]=[C:4]([Cl:13])[N:3]=1

参加物

5

反応物 3

HCID 24842Hydrazine SulfateHCID 517045Sodium AcetateHCID 89972412HCID 89972412、化合物

生成物 1

HCID 88768920HCID 88768920、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

To a suspension of 4,6-dichloro-1-hydroxy-1H-furo[3,4-c]pyridin-3-one (9.37 g) stirring in water (100 ml) was added hydrazine sulfate (10.58 ml) and sodium acetate (13.56 g). The reaction mixture was heated at reflux and stirred for 2 h. The reaction mixture was cooled to RT, diluted with water (150 ml) and extracted with EtOAc (2×75 ml). The combined organic layers were washed with saturated Na2CO3 solution and dried over Na2SO4. Evaporation to dryness gave the desired product as brown solid.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux
  3. extractionextracted with EtOAc (2×75 ml)
  4. washThe combined organic layers were washed with saturated Na2CO3 solution
  5. dry with materialdried over Na2SO4
  6. customEvaporation to dryness

出典と根拠

ORDレコード
ord-8c9942035d80453ba2ad8fdc7f24cb17
出典データセット
uspto-grants-2016_04
特許番号
US09315500B2

反応ノート

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