تفاعل #162817

معادلة التفاعل

1,3-diphenylurea

malonic acid

→

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

المردود 40.0%

المذيبات

Acetic anhydride

ظروف التفاعل

المعالجة

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
   درجة الحرارةto cool to room temperature
4. 4
   تركيزThe 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
   درجة الحرارةWhen the mixture was cooled to 40° C.
8. 8
   ترشيحthe crystals were collected by filtration
9. 9
   غسيلwashed with ethanol
10. 10
    أخرىdried

الإجراء التجريبي

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%).

المصدر