反応 #4416

反応方程式

4-(4-chlorophenyl)butyl chloride

piperazine

→

1-[4-(4-chlorophenyl)butyl]piperazine

収率 46.3%

溶媒

ethanol

反応条件

後処理

1. 1
   温度was refluxed overnight
2. 2
   その他Solvent was evaporated from the product
3. 3
   その他the residue was chromatographed twice on silica with the eluant
4. 4
   その他The first chromatography removed the bulk of the excess piperazine

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.).

出典