Реакция #5524

ord-aac0c1f80f444f1e85571cb9c0058d96

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураat reflux for 4 hours
  2. 2
    ДругоеAfter the solvent was removed
  3. 3
    workup.ADDITIONchloroform was added to the residue, which
  4. 4
    Промывкаwas washed in turn with saturated sodium bicarbonate and saturated saline
  5. 5
    Сушкаdried over anhydrous magnesium sulfate
  6. 6
    КонцентрированиеAfter the solvent was concentrated
  7. 7
    workup.ADDITIONn-hexane was added to the mixture
  8. 8
    ДругоеThen, the crystals precipitated
  9. 9
    Фильтрацияwere filtered off
  10. 10
    Промывкаwashed with n-hexane

Методика

A solution of 2-amino-6-chloropyridine (6.43 g, 50 mmoles) and ethyl bromopyruvate (9.75 g, 50 mmoles) in ethanol (150 ml) was heated at reflux for 4 hours. After the solvent was removed, chloroform was added to the residue, which was washed in turn with saturated sodium bicarbonate and saturated saline, and then dried over anhydrous magnesium sulfate. After the solvent was concentrated, n-hexane was added to the mixture. Then, the crystals precipitated were filtered off and washed with n-hexane to obtain 7.60 g of the desired product (67.6%, pale yellow crystals).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05244908uspto-grants-1993_09