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

HRID 2308391ノート

反応式

HRID 2308391 の反応式
[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

参加物

6

反応物 4

HCID 887MethanolHCID 7761Diethyl MalonateHCID 31222HydrazobenzeneHCID 10942334Sodium Methoxide

生成物 1

HCID 175611,2-Diphenyl-3,5-pyrazolidinedione収率 68.7%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4bee944250724218abd33530e74a9d17
出典データセット
uspto-grants-2004_12
特許番号
US06835845B2

反応ノート

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