Phenylhydrazine → 2-(2-Phenylhydrazono)malonic acid

HRID 1817048

반응식

HRID 1817048 반응식
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

참가 물질

4

반응물 2

HCID 7516PhenylhydrazineHCID 71317420Mesoxalicacidmonohydratedisodiumsalt

생성물 1

HCID 5486342-(2-Phenylhydrazono)malonic acid

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

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]+.

후처리

  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

출처 및 근거

ORD 기록
ord-0da3305eb5a34e4b965df07e701b012c
출처 데이터셋
uspto-grants-2009_10
특허 번호
US07598247B2

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