تفاعل #302870

معادلة التفاعل

phenylisocyanate

2-aminonicotinic acid methyl ester

→

3-phenyl-1H-pyrido[2,3-d]pyrimidine-2,4-dione

المردود 61.2%

المذيبات

pyridine

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture was refluxed for 16 hours
2. 2
   أخرىThe pyridine is was removed under reduced pressure
3. 3
   workup.ADDITIONthe residue was treated with 280 ml ethanol
4. 4
   درجة الحرارةThe mixture is refluxed for 10 minutes
5. 5
   درجة الحرارةUpon cooling down 3-phenyl-1H-pyrido[2,3-d]pyrimidine-2,4-dione
6. 6
   أخرىcrystallized from the medium
7. 7
   أخرىwas recrystallized from methoxypropanol

الإجراء التجريبي

17.22 g (144.6 mmol, 15.7 ml) phenylisocyanate was added to a suspenssion of 7.00 g (46.0 mmol) 2-aminonicotinic acid methyl ester in dry pyridine. The mixture was refluxed for 16 hours. The pyridine is was removed under reduced pressure and the residue was treated with 280 ml ethanol. The mixture is refluxed for 10 minutes. Upon cooling down 3-phenyl-1H-pyrido[2,3-d]pyrimidine-2,4-dione crystallized from the medium and was recrystallized from methoxypropanol. 6.73 g (61%) 3-phenyl-1H-pyrido[2,3-d]pyrimidine-2,4-dione was isolated (m.p. 304° C.).

المصدر