反应 #3928

ord-b5880115943c4665b571bee98c011ee9

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was refluxed for 8 hours
  2. 2
    其他The solvent was removed in vacuo, and 2N sodium hydroxide
  3. 3
    workup.ADDITIONwas added to the residue
  4. 4
    萃取The product was extracted with methylene chloride
  5. 5
    干燥the extract was dried (sodium sulfate)
  6. 6
    浓缩concentrated
  7. 7
    其他The salt was precipitated with ethereal hydrochloric acid

实验过程

A mixture of 15.0 g of 1-(4-chlorobenzyl)piperazine, 14.4 g of 1-bromo-2-chloroethane and 150 ml of tetrahydrofuran was refluxed for 8 hours. The solvent was removed in vacuo, and 2N sodium hydroxide was added to the residue. The product was extracted with methylene chloride, and the extract was dried (sodium sulfate) and concentrated. The salt was precipitated with ethereal hydrochloric acid to give 13.8 g (56% of theory) of 1-(4-chlorobenzyl)-4-(2-chloroethyl)piperazine dihydrochloride as a white crystalline solid.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04722926uspto-grants-1988_02