反応 #162817

反応方程式

1,3-diphenylurea

malonic acid

→

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

収率 40.0%

溶媒

Acetic anhydride

反応条件

後処理

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
   温度to cool to room temperature
4. 4
   濃縮The 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
   温度When the mixture was cooled to 40° C.
8. 8
   ろ過the crystals were collected by filtration
9. 9
   洗浄washed with ethanol
10. 10
    その他dried

実験手順

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%).

出典