反应详情

4-amino-2-chloro-6,7,8-trimethoxyquinazoline (1 g.) and N-(1,4-benzodioxan-2-carbonyl)piperazine (1.168 g.) were heated under reflux in n-butanol (67 ml.) with triethylamine (1.87 g.) for 24 hours. Further N-(1,4-benzodioxan-2-carbonyl)piperazine (0.026 g.) was then added and the mixture heated under reflux for an additional 30 hours. Butanol was then removed in vacuo and the residue partitioned between aqueous sodium carbonate solution and chloroform. The combined chloroform extracts were washed with water, dried (Na2SO4) and evaporated in vacuo to leave a solid (3.4 g.) which was taken up in the minimum quantity of dimethylformamide then set aside at 0° C. overnight. Ether was then added and the cloudy solution further cooled to yield 4-amino-2-[4-(1,4-benzodioxan-2-carbonyl)piperazin-1-yl]-6,7,8-trimethoxyquinazoline (0.58 g.), m.p. 269°-271° C.

1. temperaturethe mixture heated
2. temperatureunder reflux for an additional 30 hours
3. customButanol was then removed in vacuo
4. customthe residue partitioned between aqueous sodium carbonate solution and chloroform
5. washThe combined chloroform extracts were washed with water
6. dry with materialdried (Na2SO4)
7. customevaporated in vacuo
8. customto leave a solid (3.4 g.) which
9. temperaturethe cloudy solution further cooled