Реакция #1123

ord-d3878873efe84db9b86c10bc3e0d832a

Уравнение реакции

O=C([O-])O.[Na+]
sodium hydrogencarbonate
Clc1ccnc(Cl)c1Br
2,4-dichloro-3-bromopyridine
N[C@H]1CC[C@@H](c2ccccc2)CC1
cis-4-phenylcyclohexylamine
[Cl-].[NH4+]
ammonium chloride
Clc1nccc(N[C@H]2CC[C@@H](c3ccccc3)CC2)c1Br
2-Chloro-3-bromo-4-(cis-4-phenylcyclohexylamino)-pyridine

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураAfter cooling
  2. 2
    Экстракцияthe reaction product is extracted with ethyl acetate
  3. 3
    ДругоеPurification

Методика

2.27 g (10 mmol) of 2,4-dichloro-3-bromopyridine, 2.6 g (15 mmol) of cis-4-phenylcyclohexylamine and 0.1 g of ammonium chloride are heated at 120° C. for 10 hours in 10 ml of N-methylpyrrolidone. After cooling, saturated sodium hydrogencarbonate solution is added and the reaction product is extracted with ethyl acetate. Purification is carried out by column chromatography. Yield: 1.9 g (52%); m.p. 105° C.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05723450uspto-grants-1998_03