反应详情

A stirred mixture containing 13.5 g of 5-bromo-1,6-naphthyridin-2(1H)-one, 20 g of 3-methyl-1H-1,2,4-triazole and 75 ml of N-methylpyrrolidinone was heated in an oil bath at 170°-180° C. for 18 hours and then cooled to room temperature whereupon a tan solid crystallized out. The mixture was diluted by adding 125 ml of water and the separated solid was collected, washed with water, air-dried and combined with another 1.2 g sample of the same material obtained in another run starting with 2.25 g of 5-bromo-1,6-naphthyridin-2(1H)-one. The combined solids were recrystallized from dimethylformamide and dried in an oven at 95°-100° C. for three days to yield 6.1 g of 5-(3-methyl-1H-1,2,4-triazole-1-yl)-1,6-naphthyridin-2(1H)-one, m.p. >300° C.

1. temperaturewas heated in an oil bath at 170°-180° C. for 18 hours
2. customcrystallized out
3. additionThe mixture was diluted
4. additionby adding 125 ml of water
5. customthe separated solid was collected
6. washwashed with water
7. customair-dried
8. customobtained in another run
9. customThe combined solids were recrystallized from dimethylformamide
10. customdried in an oven at 95°-100° C. for three days