反応 #710481

反応方程式

2-chloro-5-chloromethyl pyridine

2-aminopyrimidine

→

1-((6-chloropyridin-3-yl)methyl)pyrimidin-2(1H)-imine hydrochloride

収率 34.0%

溶媒

DMF

反応条件

後処理

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

実験手順

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%)

出典