1H-1,2,4-Triazole, 1-[[2-(2,4-dichlorophenyl)oxiranyl]methyl]- → 1-[2-(2,4-Dichlorophenyl)-2-hydroxy-3-(1-methylimidazol-2-ylthio)-propyl]-1,2,4-triazole

HRID 2118491ノート

反応式

HRID 2118491 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1([CH2:12][N:13]2[CH:17]=[N:16][CH:15]=[N:14]2)[CH2:11][O:10]1.[SH:18][C:19]1[N:20]([CH3:24])[CH:21]=[CH:22][N:23]=1>O1CCOCC1>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]([OH:10])([CH2:11][S:18][C:19]1[N:20]([CH3:24])[CH:21]=[CH:22][N:23]=1)[CH2:12][N:13]1[CH:17]=[N:16][CH:15]=[N:14]1

参加物

4

反応物 2

HCID 104232291H-1,2,4-Triazole, 1-[[2-(2,4-dichlorophenyl)oxiranyl]methyl]-HCID 178480602HCID 178480602、化合物

生成物 1

HCID 201939451-[2-(2,4-Dichlorophenyl)-2-hydroxy-3-(1-methylimidazol-2-ylthio)-propyl]-1,2,4-triazole収率 66%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

2-(2,4-Dichlorophenyl)-2-(1H-1,2,4-triazol-1-yl-methyl)-oxirane (0.27 g, 0.001 m), and 2-mercapto-1-methylimidazole (0.228 g, 0.002 m) were heated under reflux in dioxan for 72 hours. The dioxan was then evaporated and the residue was dissolved in ethyl acetate (70 ml). This solution was washed sequentially with dilute potassium carbonate solution, dilute sodium hydroxide solution, and water dried (MgSO4) and evaporated to give an oil which crystallized on standing. Recrystallization from ethyl acetate/hexane gave the title compound 0.252 g (66%); m.p. 159°-161° C.

後処理

  1. customThe dioxan was then evaporated
  2. dissolutionthe residue was dissolved in ethyl acetate (70 ml)
  3. washThis solution was washed sequentially with dilute potassium carbonate solution, dilute sodium hydroxide solution, and water
  4. dry with materialdried (MgSO4)
  5. customevaporated
  6. customto give an oil which
  7. customcrystallized
  8. customRecrystallization from ethyl acetate/hexane

出典と根拠

ORDレコード
ord-90d982b6a7664c1e9b9f06b2340b6c9a
出典データセット
uspto-grants-1987_07
特許番号
US04678789

反応ノート

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