Dimethylformamide → 1-(4-Methoxyphenyl)-4-(4-nitrophenyl)piperazine

HRID 1154727

반응식

HRID 1154727 반응식
Cl.Cl.[CH3:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([N:11]2[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)=[CH:7][CH:6]=1.Cl[C:18]1[CH:23]=[CH:22][C:21]([N+:24]([O-:26])=[O:25])=[CH:20][CH:19]=1.C(=O)([O-])[O-].[K+].[K+].CN(C)C=O>O>[CH3:3][O:4][C:5]1[CH:6]=[CH:7][C:8]([N:11]2[CH2:16][CH2:15][N:14]([C:18]3[CH:23]=[CH:22][C:21]([N+:24]([O-:26])=[O:25])=[CH:20][CH:19]=3)[CH2:13][CH2:12]2)=[CH:9][CH:10]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 74741-Chloro-4-nitrobenzeneHCID 11430Potassium CarbonateHCID 27237001-(4-Methoxyphenyl)-piperazine, dihydrochloride

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 13.4 parts of 1-(4-methoxyphenyl)piperazine dihydrochloride, 7.9 parts of 1-chloro-4-nitrobenzene, 10 parts of potassium carbonate and 90 parts of N,N-dimethylformamide is stirred and refluxed overnight. The reaction mixture is diluted with water and the product is extracted twice with trichloromethane. The combined extracts are dried, filtered and evaporated. The residue is triturated in 4-methyl-2-pentanone. The product is filtered off and crystallized from 1,4-dioxane, yielding 10.5 parts (67%) of 1-(4-methoxyphenyl)-4-(4-nitrophenyl)piperazine; mp. 195.1° C.

후처리

  1. temperaturerefluxed overnight
  2. extractionthe product is extracted twice with trichloromethane
  3. customThe combined extracts are dried
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue is triturated in 4-methyl-2-pentanone
  7. filtrationThe product is filtered off
  8. customcrystallized from 1,4-dioxane

출처 및 근거

ORD 기록
ord-5a7c8710c45e4270a123e201951785e5
출처 데이터셋
uspto-grants-1984_12
특허 번호
US04490530

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