Tetrahydrofuran → 1-Diallylcarbamoyl-3-n-butylsulphinyl-1,2,4-triazole

HRID 1606061노트

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HRID 1606061 반응식
[CH2:1]([S:5]([C:7]1[N:11]=[CH:10][NH:9][N:8]=1)=[O:6])[CH2:2][CH2:3][CH3:4].[CH2:12]([N:15]([CH2:19][CH:20]=[CH2:21])[C:16](Cl)=[O:17])[CH:13]=[CH2:14].O1CCCC1>C(N(CC)CC)C>[CH2:12]([N:15]([CH2:19][CH:20]=[CH2:21])[C:16]([N:9]1[CH:10]=[N:11][C:7]([S:5]([CH2:1][CH2:2][CH2:3][CH3:4])=[O:6])=[N:8]1)=[O:17])[CH:13]=[CH2:14]

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 3449313Diallylcarbamyl chlorideHCID 1784555543-Butylsulphinyl-1,2,4-triazole

생성물 1

HCID 203551101-Diallylcarbamoyl-3-n-butylsulphinyl-1,2,4-triazole

시약·촉매·용매 1

HCID 8471Triethylamine용매

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온도
100 °C

실험 절차

A mixture of 5.2 g. 3-butylsulphinyl-1,2,4-triazole, 6.0 g. diallylcarbamoyl chloride, 25 ml. dry tetrahydrofuran and 7.5 ml. dry triethylamine was refluxed under anhydrous conditions for 2 hours. The reaction mixture was filtered to remove triethylamine hydrochloride and the filtrate distilled under reduced pressure to remove solvent. Finally the residue was maintained at 100°C./0.5 mm. for 30 minutes in order to remove all traces of volatile material from the product. The product, 1-diallylcarbamoyl-3-n-butylsulphinyl-1,2,4-triazole, was obtained as an oil, nD26 1.5277. Elemental analysis satisfactory.

후처리

  1. additionA mixture of 5.2 g
  2. filtrationThe reaction mixture was filtered
  3. customto remove triethylamine hydrochloride
  4. distillationthe filtrate distilled under reduced pressure
  5. customto remove solvent
  6. customfor 30 minutes in order to remove all traces of volatile material from the product

출처 및 근거

ORD 기록
ord-429090962a8d453b87e9b6a1fbb619c9
출처 데이터셋
uspto-grants-1976_04
특허 번호
US03952001

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