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Hydrogen Peroxide → 1-Dipropylcarbamoyl-3-propylsulphinyl-1,2,4-triazole

HRID 371600
ノート
印刷プレビュー

反応式

HRID 371600 の反応式
[CH2:1]([N:4]([CH2:16][CH2:17][CH3:18])[C:5]([N:7]1[CH:11]=[N:10][C:9]([S:12][CH2:13][CH2:14][CH3:15])=[N:8]1)=[O:6])[CH2:2][CH3:3].[OH:19]O>C(O)(=O)C>[CH2:16]([N:4]([CH2:1][CH2:2][CH3:3])[C:5]([N:7]1[CH:11]=[N:10][C:9]([S:12]([CH2:13][CH2:14][CH3:15])=[O:19])=[N:8]1)=[O:6])[CH2:17][CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 784Hydrogen PeroxideHCID 203549191-Dipropylcarbamoyl-3-propylthio-1,2,4-triazole

生成物 1

HCID 203551191-Dipropylcarbamoyl-3-propylsulphinyl-1,2,4-triazole

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 13.5 g. 1-dipropylcarbamoyl-3-propylthio-1,2,4-triazole and 100 vol. hydrogen peroxide solution (5.7 ml., 1.0 molecular proportion) in 450 ml. glacial acetic acid was kept at room temperature for 14 days. The resulting solution was evaporated to dryness under reduced pressure and the residual oil was dissolved in methylene dichloride. The resulting solution was washed successively with 0.5N sodium hydroxide solution, and 0.5N hydrochloric acid. Solvent was removed from the solution by distillation under reduced pressure to give a residual oil which solidified on cooling. The solid product was recrystallized from benzene/petroleum ether, b.p. 40° - 60° C. to give 1-dipropylcarbamoyl-3-propylsulphinyl-1,2,4-triazole, m.p. 51° - 52.5° C. Elemental analysis satisfactory.

後処理

  1. customThe resulting solution was evaporated to dryness under reduced pressure
  2. dissolutionthe residual oil was dissolved in methylene dichloride
  3. washThe resulting solution was washed successively with 0.5N sodium hydroxide solution, and 0.5N hydrochloric acid
  4. customSolvent was removed from the solution by distillation under reduced pressure
  5. customto give a residual oil which
  6. temperatureon cooling
  7. customThe solid product was recrystallized from benzene/petroleum ether, b.p. 40° - 60° C.

出典と根拠

ORDレコード
ord-c69623ee67e7461984a546ce945f9759
出典データセット
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04087269

反応ノート

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