Sodium Hydroxide → HCID 86683166、化合物

HRID 920948ノート

反応式

HRID 920948 の反応式
C([NH:4]/[N:5]=[CH:6]/[C:7]1[CH:17]=[N:16][CH:15]=[C:14]([Cl:18])[C:8]=1[C:9](OCC)=[O:10])(=O)C.[OH-].[Na+].C([O-])(O)=O.[Na+]>O1CCOCC1>[Cl:18][C:14]1[C:8]2[C:9](=[O:10])[NH:4][N:5]=[CH:6][C:7]=2[CH:17]=[N:16][CH:15]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 140606546HCID 140606546、化合物

生成物 1

HCID 86683166HCID 86683166、化合物収率 16.9%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

(E)-ethyl 3-((2-acetylhydrazono)methyl)-5-chloroisonicotinate (220 mg, 0.816 mmol) and aq. NaOH solution (3.26 mg, 0.082 mmol, 2 molar) in 5 mL of dioxane were stirred in a microwave at 165° C. for 60 min. Then the reaction mixture was basified by addition of aq. NaHCO3 and extracted with DCM. The organic phase was washed with brine, dried and concentrated. The crude title compound was purified by chromatography (eluent: DCM/methanol) to give 25 mg (16.88%) of the title compound as beige solid.

後処理

  1. extractionextracted with DCM
  2. washThe organic phase was washed with brine
  3. customdried
  4. concentrationconcentrated
  5. customThe crude title compound was purified by chromatography (eluent: DCM/methanol)

出典と根拠

ORDレコード
ord-c902341448284337a4735ac2bbe08a13
出典データセット
uspto-grants-2016_03
特許番号
US09273068B2

反応ノート

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