Phenylhydrazine → 2-(2-Phenylhydrazono)malonic acid

HRID 264026

反応式

HRID 264026 の反応式
O.O=[C:3]([C:7]([OH:9])=[O:8])[C:4]([OH:6])=[O:5].[C:10]1([NH:16][NH2:17])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>C(O)C.O>[C:10]1([NH:16][N:17]=[C:3]([C:7]([OH:9])=[O:8])[C:4]([OH:6])=[O:5])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

5

反応物 2

HCID 7516PhenylhydrazineHCID 20057180Ketomalonic acid hydrate

生成物 1

HCID 5486342-(2-Phenylhydrazono)malonic acid収率 94.5%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a vigorously stirred solution of ketomalonic acid monohydrate (29.33 g) in ethanol (140 ml) and water (300 ml) at ambient temperature was added phenylhydrazine (23.3 g) dropwise over a 40 minute period. The resultant slurry was stirred overnight at ambient temperature. The solid was separated by filtration, washed sucessively with cold water (100 ml) and ethanol (25 ml) and air dried. Subsequent drying was performed at 75° C. overnight in a vacuum oven to give the title compound as a yellow solid (42.38 g). 1H (300 MHz, DMSO-d6): d 7.12(t, 1H), 7.35-7.48(m, 4H); m.p.: 155°-157° C. (dec).

後処理

  1. customThe solid was separated by filtration
  2. washwashed sucessively with cold water (100 ml) and ethanol (25 ml) and air
  3. customdried
  4. customSubsequent drying
  5. waitwas performed at 75° C. overnight in a vacuum oven

出典と根拠

ORDレコード
ord-049ebd35499f461b92cb1d39c5fd29d3
出典データセット
uspto-grants-1997_07
特許番号
US05646140

関連ノート

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