반응 #44705

반응 방정식

phosphoryl chloride

3-(2-amino-6-oxo-1,6-dihydropyrimidin-4-yl)benzonitrile

N,N-diethylaniline

→

title compound

3-(2-Amino-6-chloropyrimidin-4-yl)benzonitrile

반응 조건

후처리

1. 1
   workup.WAITover a period of a further hour
2. 2
   온도The mixture is then heated at RF for one hour
3. 3
   온도to cool to RT
4. 4
   추출The mixture is extracted twice with ethyl acetate
5. 5
   기타the solvent is removed under reduced pressure
6. 6
   온도With ice-cooling
7. 7
   workup.ADDITIONthe solution is neutralized by addition of conc. sodium hydroxide solution
8. 8
   workup.ADDITIONSaturated sodium carbonate solution is added
9. 9
   여과The precipitate is filtered off with suction
10. 10
    세척washed with water

실험 절차

2.00 g (9.42 mmol) of 3-(2-amino-6-oxo-1,6-dihydropyrimidin-4-yl)benzonitrile (from example LV) are suspended in 10 ml of phosphoryl chloride. Over a period of one hour, 180 mg (1.23 mmol) of N,N-diethylaniline are added dropwise, and over a period of a further hour, the mixture is heated to 115° C. The mixture is then heated at RF for one hour. The mixture is allowed to cool to RT and poured into ice water. The mixture is extracted twice with ethyl acetate and the solvent is removed under reduced pressure. The residue is suspended in water. With ice-cooling, the solution is neutralized by addition of conc. sodium hydroxide solution. Saturated sodium carbonate solution is added, and the mixture is stirred at RT overnight. The precipitate is filtered off with suction and washed with water. This gives the title compound.

출처