Реакция #710481

ord-af4cb05f4ccf4c029efb5271f7ccee41

Уравнение реакции

ClCc1ccc(Cl)nc1
2-chloro-5-chloromethyl pyridine
Nc1ncccn1
2-aminopyrimidine
Cl.N=c1ncccn1Cc1ccc(Cl)nc1
1-((6-chloropyridin-3-yl)methyl)pyrimidin-2(1H)-imine hydrochloride
Выход 34.0%

Реагенты

Нет

Растворители

Условия реакции

Температура
80°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеwas returned to room temperature
  2. 2
    workup.DISTILLATIONto distill off DMF under reduced pressure
  3. 3
    workup.ADDITIONDiethyl ether was added
  4. 4
    Другоеthus crystallization
  5. 5
    Другоеwas occurred on the wall surface of an eggplant flask
  6. 6
    ДругоеDiethyl ether was removed by decantation
  7. 7
    Другоеdried well

Методика

300 mg (1.86 mmol) of 2-chloro-5-chloromethyl pyridine was dissolved in 6 ml of anhydrous DMF, 118 mg (1.24 mmol) of 2-aminopyrimidine was added thereto, and the resulting mixture was stirred at 80° C. for 8 hours. After the reaction was completed, the reaction solution was returned to room temperature to distill off DMF under reduced pressure. Diethyl ether was added thereto, and thus crystallization was occurred on the wall surface of an eggplant flask. Diethyl ether was removed by decantation and dried well to obtain 1-((6-chloropyridin-3-yl)methyl)pyrimidin-2(1H)-imine hydrochloride. Amount obtained 107 mg (yield 34%)

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09301525B2uspto-grants-2016_04