반응 #710481

ord-af4cb05f4ccf4c029efb5271f7ccee41

반응 방정식

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
수율 34.0%

용매

반응 조건

온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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%)

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09301525B2uspto-grants-2016_04