반응 #710481
ord-af4cb05f4ccf4c029efb5271f7ccee41
반응 방정식
2-chloro-5-chloromethyl pyridine
2-aminopyrimidine
→
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
- 1기타was returned to room temperature
- 2workup.DISTILLATIONto distill off DMF under reduced pressure
- 3workup.ADDITIONDiethyl ether was added
- 4기타thus crystallization
- 5기타was occurred on the wall surface of an eggplant flask
- 6기타Diethyl ether was removed by decantation
- 7기타dried 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%)