반응 #459823

반응 방정식

4,6-dichloro-2-(1-cyano-1-methylethylamino)-5-pyrimidinecarbonitrile

isopropylamine

→

4-chloro-2-(1-cyano-1-methylethylamino)-6-isopropylamino-5-pyrimidinecarbonitrile

수율 48.6%

용매

acetone

반응 조건

후처리

1. 1
   기타The acetone was removed under reduced pressure
2. 2
   추출the reaction mixture was extracted with a mixture of diethyl ether and water
3. 3
   기타The organic layer was separated
4. 4
   건조dried over magnesium sulfate
5. 5
   여과The solution was filtered
6. 6
   기타the filtrate was evaporated under reduced pressure
7. 7
   기타yielding a residue
8. 8
   기타The residue was recrystallized from methylcyclohexane

실험 절차

To a stirred solution of 5.1 grams of 4,6-dichloro-2-(1-cyano-1-methylethylamino)-5-pyrimidinecarbonitrile in 100 ml of acetone, 2.3 grams of isopropylamine was added dropwise. The reaction mixture was then stirred at room temperature for 16 hours. The acetone was removed under reduced pressure, and the reaction mixture was extracted with a mixture of diethyl ether and water. The organic layer was separated and dried over magnesium sulfate. The solution was filtered, and the filtrate was evaporated under reduced pressure, yielding a residue. The residue was recrystallized from methylcyclohexane to give 2.7 grams of 4-chloro-2-(1-cyano-1-methylethylamino)-6-isopropylamino-5-pyrimidinecarbonitrile; mp, 144°-147°.

출처