Piperazine → Piperazine,1-[4-(4-chlorophenyl)butyl]-

HRID 4320

反応式

HRID 4320 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][CH2:10][CH2:11]Cl)=[CH:4][CH:3]=1.[NH:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][CH2:10][CH2:11][N:13]2[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]2)=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 4837PiperazineHCID 200827321-Chloro-4-(4-chlorobutyl)benzene

生成物 1

HCID 14097058Piperazine,1-[4-(4-chlorophenyl)butyl]-収率 46.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 26.4 g of 4-(4-chlorophenyl)butyl chloride, 86.1 g of anhydrous piperazine and 250 ml of reagent ethanol was refluxed overnight. Solvent was evaporated from the product and the residue was chromatographed twice on silica with the eluant being CH2Cl2 /CH3OH/ammonium hydroxide (45:5:1). The first chromatography removed the bulk of the excess piperazine, the second provided 15.2 g of 1-[4-(4-chlorophenyl)butyl]piperazine as a colorless oil which solidified on standing (m.p. 139°-145° C.).

後処理

  1. temperaturewas refluxed overnight
  2. customSolvent was evaporated from the product
  3. customthe residue was chromatographed twice on silica with the eluant
  4. customThe first chromatography removed the bulk of the excess piperazine

出典と根拠

ORDレコード
ord-81005d9a5e474ae9811ee087317133f2
出典データセット
uspto-grants-1988_02
特許番号
US04725597

関連ノート

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