1H-1,2,4-Triazole → 1-[2-(2,4-dichlorophenyl)-2,2-dimethoxyethyl]-1H-1,2,4-triazole

HRID 971644

反応式

HRID 971644 の反応式
[NH:1]1[CH:5]=[N:4][CH:3]=[N:2]1.[H-].[Na+].Br[CH2:9][C:10]([C:15]1[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][C:16]=1[Cl:22])([O:13][CH3:14])[O:11][CH3:12]>CN(C)C=O>[Cl:22][C:16]1[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:15]=1[C:10]([O:13][CH3:14])([O:11][CH3:12])[CH2:9][N:1]1[CH:5]=[N:4][CH:3]=[N:2]1

参加物

5

反応物 3

HCID 92571H-1,2,4-TriazoleHCID 24758Sodium hydrideHCID 127058821-(2-Bromo-1,1-dimethoxyethyl)-2,4-dichlorobenzene

生成物 1

HCID 159177871-[2-(2,4-dichlorophenyl)-2,2-dimethoxyethyl]-1H-1,2,4-triazole収率 44%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a stirred mixture of 19 parts of 1H-1,2,4-triazole and 225 parts of N,N-dimethylformamide are added 8.4 parts of sodium hydride dispersion 78% and stirring is continued till foaming has ceased. Then there are added 29 parts of 1-(2-bromo-1,1-dimethoxyethyl)-2,4-dichlorobenzene and the whole is stirred and refluxed overnight. The reaction mixture is cooled, poured onto water and the product is extracted twice with 2,2'-oxybispropane. The combined extracts are washed with water, dried, filtered and evaporated. The residue is crystallized from petroleumether (activated charcoal), yielding 12.1 parts (44%) of 1-[2-(2,4-dichlorophenyl)-2,2-dimethoxyethyl]-1H-1,2,4-triazole; mp. 87.7° C.

後処理

  1. stirringthe whole is stirred
  2. temperaturerefluxed overnight
  3. temperatureThe reaction mixture is cooled
  4. additionpoured onto water
  5. extractionthe product is extracted twice with 2,2'-oxybispropane
  6. washThe combined extracts are washed with water
  7. customdried
  8. filtrationfiltered
  9. customevaporated
  10. customThe residue is crystallized from petroleumether (activated charcoal)

出典と根拠

ORDレコード
ord-5de22553ff3c40d6b73e14f82bde9731
出典データセット
uspto-grants-1979_07
特許番号
US04160838

関連ノート

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