Diethylcarbamoyl chloride → 1-Diethylcarbamoyl-3-diallylsulphamoyl-1,2,4-triazole

HRID 1606096

反応式

HRID 1606096 の反応式
[CH2:1]([N:4]([CH2:13][CH:14]=[CH2:15])[S:5]([C:8]1[N:12]=[CH:11][NH:10][N:9]=1)(=[O:7])=[O:6])[CH:2]=[CH2:3].[CH2:16]([N:18]([CH2:22][CH3:23])[C:19](Cl)=[O:20])[CH3:17].C(N(CC)CC)C>O1CCCC1>[CH2:16]([N:18]([CH2:22][CH3:23])[C:19]([N:10]1[CH:11]=[N:12][C:8]([S:5](=[O:7])(=[O:6])[N:4]([CH2:1][CH:2]=[CH2:3])[CH2:13][CH:14]=[CH2:15])=[N:9]1)=[O:20])[CH3:17]

参加物

5

反応物 3

HCID 6916Diethylcarbamoyl chlorideHCID 8471TriethylamineHCID 178457344HCID 178457344、化合物

生成物 1

HCID 213242681-Diethylcarbamoyl-3-diallylsulphamoyl-1,2,4-triazole

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 6.9 g. 3-diallylsulphamoyl-1,2,4-triazole, 4.5 g. diethylcarbamoyl chloride, 6 ml. triethylamine and 25 ml. dry tetrahydrofuran was refluxed under anhydrous conditions for 1.5 hours. The cooled reaction mixture was filtered to remove triethylamine hydrochloride and the filtrate was evaporated to remove solvent. The solid residue was recrystallized from petroleum ether, b.p. 60° - 80°C., to give 1-diethylcarbamoyl-3-diallylsulphamoyl-1,2,4-triazole, m.p. 49° - 51°C. Elemental analysis satisfactory.

後処理

  1. additionA mixture of 6.9 g
  2. customThe cooled reaction mixture
  3. filtrationwas filtered
  4. customto remove triethylamine hydrochloride
  5. customthe filtrate was evaporated
  6. customto remove solvent
  7. customThe solid residue was recrystallized from petroleum ether, b.p. 60° - 80°C.

出典と根拠

ORDレコード
ord-7dce2d67e7c045ad84a8765449c8b1b8
出典データセット
uspto-grants-1976_04
特許番号
US03952001

関連ノート

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