Реакция #5524
ord-aac0c1f80f444f1e85571cb9c0058d96
Уравнение реакции
Реагенты
Нет
Растворители
Условия реакции
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1Температураat reflux for 4 hours
- 2ДругоеAfter the solvent was removed
- 3workup.ADDITIONchloroform was added to the residue, which
- 4Промывкаwas washed in turn with saturated sodium bicarbonate and saturated saline
- 5Сушкаdried over anhydrous magnesium sulfate
- 6КонцентрированиеAfter the solvent was concentrated
- 7workup.ADDITIONn-hexane was added to the mixture
- 8ДругоеThen, the crystals precipitated
- 9Фильтрацияwere filtered off
- 10Промывкаwashed 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).