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

HRID 1634001

반응식

HRID 1634001 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-85dba744142a49b1a8696df351e74ca4
출처 데이터셋
uspto-grants-2003_01
특허 번호
US06506507B1

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