반응 #162817

반응 방정식

1,3-diphenylurea

malonic acid

→

1,3-diphenyl-pyrimidine-2,4,6-trione

수율 40.0%

용매

Acetic anhydride

반응 조건

후처리

1. 1
   workup.ADDITIONwas added under a nitrogen atmosphere
2. 2
   workup.STIRRINGThe mixture was stirred at 100° C. for 1.5 hrs
3. 3
   온도to cool to room temperature
4. 4
   농축The reaction mixture was concentrated under reduced pressure
5. 5
   workup.ADDITIONEthanol (500 ml) was added to the residue
6. 6
   workup.STIRRINGthe mixture was stirred at 90° C
7. 7
   온도When the mixture was cooled to 40° C.
8. 8
   여과the crystals were collected by filtration
9. 9
   세척washed with ethanol
10. 10
    기타dried

실험 절차

Acetic anhydride (290 ml) was added to 1,3-diphenylurea 18 (148 g), malonic acid 4 (81.6 g) was added under a nitrogen atmosphere, and the mixture was stirred at 90° C. for 3 hrs. The mixture was stirred at 100° C. for 1.5 hrs and allowed to cool to room temperature. The reaction mixture was concentrated under reduced pressure. Ethanol (500 ml) was added to the residue, and the mixture was stirred at 90° C. When the mixture was cooled to 40° C., the crystals were collected by filtration, washed with ethanol and dried to give 1,3-diphenyl-pyrimidine-2,4,6-trione 19 (78.0 g, yield 40%).

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