반응 #3576

반응 방정식

sodium hydride

4-pyridylaceto-nitrile hydrochloride

4-pyridylacetonitrile

sodium 2-ethoxyethoxide

2,4-diamino-5-pyrimidinecarboxaldehyde

→

title compound

6-Pyridin-4-yl-pyrido[2,3-d]pyrimidine-2,7-diamine

용매

2-ethoxyethanol

2-ethoxyethanol

반응 조건

후처리

1. 1
   workup.STIRRINGthe mixture was stirred at room temperature for 30 minutes
2. 2
   온도The resulting mixture was heated
3. 3
   온도at reflux for 2 hours
4. 4
   온도cooled
5. 5
   세척the insoluble product washed with diethylether and ethyl acetate

실험 절차

To cooled (0° C.) 2-ethoxyethanol (13 mL) was added portionwise 0.30 g of sodium hydride (60% in mineral oil), and the suspension was stirred for 10 minutes. To this suspension was added 1.06 g of 4-pyridylaceto-nitrile hydrochloride, and the mixture was stirred at room temperature for 30 minutes. The neutralized solution of 4-pyridylacetonitrile in 2-ethoxyethanol was added to a reaction mixture containing sodium 2-ethoxyethoxide (prepared from 0.11 g of sodium hydride and 4.76 mL of 2-ethoxyethanol) and 0.9 g of 2,4-diamino-5-pyrimidinecarboxaldehyde. The resulting mixture was heated at reflux for 2 hours, cooled, and the insoluble product washed with diethylether and ethyl acetate to afford the title compound; mp >340° C.; MS(CI).

출처