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

HRID 4320

반응식

HRID 4320 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-81005d9a5e474ae9811ee087317133f2
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04725597

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