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

HRID 371600
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HRID 371600 반응식
[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]
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참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-c69623ee67e7461984a546ce945f9759
출처 데이터셋
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04087269

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