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

HRID 1154727

反応式

HRID 1154727 の反応式
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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5a7c8710c45e4270a123e201951785e5
出典データセット
uspto-grants-1984_12
特許番号
US04490530

関連ノート

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