2-Hydrazinopyridine → HCID 178515860、化合物

HRID 476200

反応式

HRID 476200 の反応式
O=[C:2]([CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[CH2:3][C:4]([O:6]CC)=O.[NH:16]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][N:19]=1)[NH2:17]>C(O)C>[CH2:9]([C:2]1[CH:3]=[C:4]([OH:6])[N:16]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][N:19]=2)[N:17]=1)[C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1

参加物

4

反応物 2

HCID 786452-HydrazinopyridineHCID 225855Ethyl 3-oxo-4-phenylbutanoate

生成物 1

HCID 178515860HCID 178515860、化合物収率 30.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

Compound 2a (1.03 g, 5.0 mmol) prepared in Step 1 of Example A-1 was charged in a 25 mL round-bottom flask and dissolved in 6 mL of ethanol. A solution of 2-hydrazinopyridine (0.55 g, 5.0 mmol, manufactured by Aldrich) in 5 mL of ethanol at 50° C. was gradually added thereto over 30 minutes, followed by reaction for 1 hour. After completion of the reaction was confirmed by TLC, the reaction solution was concentrated by evaporation, extracted with ethyl acetate, washed with saturated brine, dried over anhydrous sodium sulfate, concentrated, and then purified by column chromatography [n-Hex/EtOAc=3/1 (v/v)] to afford a compound of 3-benzyl-1-(pyridin-2-yl)-1H-pyrazol-5-ol (3a).

後処理

  1. customfollowed by reaction for 1 hour
  2. concentrationthe reaction solution was concentrated by evaporation
  3. extractionextracted with ethyl acetate
  4. washwashed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated
  7. custompurified by column chromatography [n-Hex/EtOAc=3/1 (v/v)]

出典と根拠

ORDレコード
ord-8c28fcb7cca348d3bd20de67b4acdc17
出典データセット
uspto-grants-2014_01
特許番号
US08637674B2

関連ノート

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