1-Chloro-4-nitrobenzene → 1-(4-Methoxyphenyl)-4-(4-nitrophenyl)piperazine

HRID 266060

反応式

HRID 266060 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)=[CH:5][CH:4]=1.Cl[C:16]1[CH:21]=[CH:20][C:19]([N+:22]([O-:24])=[O:23])=[CH:18][CH:17]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O.O>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([N:9]2[CH2:14][CH2:13][N:12]([C:16]3[CH:21]=[CH:20][C:19]([N+:22]([O-:24])=[O:23])=[CH:18][CH:17]=3)[CH2:11][CH2:10]2)=[CH:7][CH:8]=1

参加物

6

反応物 3

HCID 74741-Chloro-4-nitrobenzeneHCID 11430Potassium CarbonateHCID 2697221-(4-Methoxyphenyl)piperazine

生成物 1

HCID 51346571-(4-Methoxyphenyl)-4-(4-nitrophenyl)piperazine収率 67%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 1-(4-methoxyphenyl)piperazine dihyclrochloride (0.050 mol), 1-chloro-4-nitrobenzene (0.050 mol) and potassium carbonate (10.0 g) in N,N-dimethylform-amide (100 ml) was stirred and refluxed overnight. The reaction mixture was diluted with water and extracted twice with trichloromethane. The organic layers were combined, dried (MgSO4), filtered and evaporated in vacuum. The residue was successively triturated in 4-methyl-2-pentanone and recrystallized from 1,4-dioxane. The product was filtered off and dried, yielding 10.5 g (67%) of 1-(4-methoxyphenyl)-4-(4-nitrophenyl)-piperazine; mp. 195.1° C. (interm. 1).

後処理

  1. temperaturerefluxed overnight
  2. extractionextracted twice with trichloromethane
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customevaporated in vacuum
  6. customThe residue was successively triturated in 4-methyl-2-pentanone
  7. customrecrystallized from 1,4-dioxane
  8. filtrationThe product was filtered off
  9. customdried

出典と根拠

ORDレコード
ord-8ff926236b0348718f1a82d2869d7a1d
出典データセット
uspto-grants-1997_07
特許番号
US05650411

関連ノート

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