Реакция #3928

ord-b5880115943c4665b571bee98c011ee9

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураwas refluxed for 8 hours
  2. 2
    ДругоеThe solvent was removed in vacuo, and 2N sodium hydroxide
  3. 3
    workup.ADDITIONwas added to the residue
  4. 4
    ЭкстракцияThe product was extracted with methylene chloride
  5. 5
    Сушкаthe extract was dried (sodium sulfate)
  6. 6
    Концентрированиеconcentrated
  7. 7
    ДругоеThe salt was precipitated with ethereal hydrochloric acid

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04722926uspto-grants-1988_02