反応 #3928

ord-b5880115943c4665b571bee98c011ee9

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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.

出典

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