Phenylhydrazine → 2-(2-Phenylhydrazono)malonic acid

HRID 1875465

反応式

HRID 1875465 の反応式
O.[C:2]([O-:9])(=[O:8])[C:3]([C:5]([O-:7])=[O:6])=O.[Na+].[Na+].[C:12]1([NH:18][NH2:19])[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>Cl>[C:12]1([NH:18][N:19]=[C:3]([C:5]([OH:7])=[O:6])[C:2]([OH:9])=[O:8])[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

参加物

4

反応物 2

HCID 7516PhenylhydrazineHCID 71317420Mesoxalicacidmonohydratedisodiumsalt

生成物 1

HCID 5486342-(2-Phenylhydrazono)malonic acid

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

Sodium mesoxalate monohydrate (5.00 g, 27.8 mmol) was dissolved in 1 M hydrochloric acid (50 ml) to give a colourless cloudy solution. Phenylhydrazine (3.00 g, 2.72 ml, 27.8 mmol) was added dropwise at room temperature to the stirred mixture. A yellow precipitate formed, was collected by filtration after 90 min and washed with water (50 ml). The filter cake was triturated with ethyl acetate/hexane [1:1], filtered and dried under vacuum. The title compound was isolated as a yellow powder (4.74 g, 22.7 mmol, 82%). LCMS: m/z 207 [M−H]+.

後処理

  1. customto give a colourless cloudy solution
  2. customA yellow precipitate formed
  3. filtrationwas collected by filtration after 90 min
  4. washwashed with water (50 ml)
  5. customThe filter cake was triturated with ethyl acetate/hexane [1:1]
  6. filtrationfiltered
  7. customdried under vacuum

出典と根拠

ORDレコード
ord-4ebe665daa844f118a65bb9244cb9d08
出典データセット
uspto-grants-2012_11
特許番号
US08309552B2

関連ノート

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