Phenylhydrazine → 2-(2-Phenylhydrazono)malonic acid

HRID 264026

반응식

HRID 264026 반응식
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

참가 물질

5

반응물 2

HCID 7516PhenylhydrazineHCID 20057180Ketomalonic acid hydrate

생성물 1

HCID 5486342-(2-Phenylhydrazono)malonic acid수율 94.5%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-049ebd35499f461b92cb1d39c5fd29d3
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05646140

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