反应 #4416
ord-81005d9a5e474ae9811ee087317133f2
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度was refluxed overnight
- 2其他Solvent was evaporated from the product
- 3其他the residue was chromatographed twice on silica with the eluant
- 4其他The first chromatography removed the bulk of the excess piperazine
实验过程
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.).