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

HRID 266060

반응식

HRID 266060 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 51346571-(4-Methoxyphenyl)-4-(4-nitrophenyl)piperazine수율 67%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-8ff926236b0348718f1a82d2869d7a1d
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05650411

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