反应详情

To 35 ml. of isoamyl alcohol were added 1.50 g. (5.47 mmole) of 4-amino-2,6-dichloro-7,8-dimethoxyquinazoline and 1.11 g. (6.02 mmole) of 1-(2-tetrahydrofuroyl)piperazine and the mixture was heated at reflux under a nitrogen atmosphere for 1.5 hours. The mixture was cooled, 20 ml. of ethyl ether was added and the resulting mixture stirred at room temperature overnight. It was then cooled in ice and the precipitated solid collected by filtration. The crude material was recrystallized once from a mixture of isopropanol, methanol and ethyl ether. The recrystallized material was dissolved in water made strongly alkaline with sodium hydroxide solution while stirring, the precipitated brownish solid collected by filtration, dried, decolorized with activated carbon and recrystallized from isopropanol/ethyl ether to obtain 0.38 g. of yellow solid, M.P. 192°-193° C.

1. temperatureat reflux under a nitrogen atmosphere for 1.5 hours
2. temperatureThe mixture was cooled
3. temperatureIt was then cooled in ice
4. filtrationthe precipitated solid collected by filtration
5. customThe crude material was recrystallized once from a mixture of isopropanol, methanol and ethyl ether
6. dissolutionThe recrystallized material was dissolved in water
7. stirringwhile stirring
8. filtrationthe precipitated brownish solid collected by filtration
9. customdried
10. customrecrystallized from isopropanol/ethyl ether
11. customto obtain 0.38 g