Methanol → 1,2-Diphenyl-3,5-pyrazolidinedione

HRID 2308146

반응식

HRID 2308146 반응식
[C:1]([O:9]CC)(=O)[CH2:2][C:3]([O:5]CC)=O.[C:12]1([NH:18][NH:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.CO.C[O-].[Na+]>C(O)CCC>[C:20]1([N:19]2[C:1](=[O:9])[CH2:2][C:3](=[O:5])[N:18]2[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1

참가 물질

6

반응물 4

HCID 887MethanolHCID 7761Diethyl MalonateHCID 31222HydrazobenzeneHCID 10942334Sodium Methoxide

생성물 1

HCID 175611,2-Diphenyl-3,5-pyrazolidinedione수율 68.7%

시약·촉매·용매 1

HCID 2631-Butanol용매

반응 조건

온도
100 °C

실험 절차

Three point six five (3.65) grams (22.8 mmol) of diethyl malonate and 4.00 g (21.7 mmol) of 1,2-diphenylhydrazine were dissolved in 10 ml of n-butanol, then 4.61 g (23.9 mmol) of a 28% methanol solution of sodium methoxide was added thereto, and the reaction system was heated at 100° C. for 10 hours. Subsequently, the solvent was distilled off under reduced pressure, 10 ml of water was added thereto and stirred, and then the reaction solution was filtered. An activated carbon was added to the recovered filtrate and stirred for 30 minutes. After stirring, the solution was filtered again to recover the filtrate. Four (4) ml of hydrochloric acid was added to the filtrate, and the precipitated solid was recovered by filtration. Thus, 3.76 g (yield: 60%) of 1,2-diphenyl-3,5-pyrazolidinedione was obtained.

후처리

  1. distillationSubsequently, the solvent was distilled off under reduced pressure, 10 ml of water
  2. additionwas added
  3. filtrationthe reaction solution was filtered
  4. additionAn activated carbon was added to the recovered filtrate
  5. stirringstirred for 30 minutes
  6. stirringAfter stirring
  7. filtrationthe solution was filtered again
  8. customto recover the filtrate
  9. additionFour (4) ml of hydrochloric acid was added to the filtrate
  10. filtrationthe precipitated solid was recovered by filtration

출처 및 근거

ORD 기록
ord-d985e09a4d3548eb92a196bb6bf32701
출처 데이터셋
uspto-grants-2004_12
특허 번호
US06835474B2

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