反应详情

温度

140 °C

Preparation of 2,5,7-Trimethyl-3-(2-methylsulfamoyl-phenyl)-4-oxo-3,4-dihydro-quinazoline-6-carboxylic acid ethyl ester: A heterogeneous mixture of 4-Acetylamino-2,6-dimethyl-isophthalic acid 1-ethyl ester (5.39 g, 1.95 mmol), 2-amino-N-methyl-benzenesulfonamide (3.63 g, 1.95 mmol), and phosphorus trichloride (8.5 mL, 9.7 mmol) in toluene (220 mL) was heated at 140° C. (oil bath temperature) for 3.5 h. The reaction mixture was allowed to cool to room temperature and then evaporated in vacuo. Sufficient ethyl acetate was added to dissolve the residue and the solution was washed with saturated aqueous sodium hydrogen carbonate then brine, dried (Na2SO4) and evaporated in vacuo. Trituration of the residue with dichloromethane gave a white solid, which was removed by filtration. Evaporation of the filtrate solution followed by trituration with ethyl acetate provided a second crop of white solid. The evaporation-trituration procedure was repeated to give two further crops of white solid. The combined white solids were washed with ether and dried in vacuo to provide the title compound.

1. temperatureto cool to room temperature
2. customevaporated in vacuo
3. additionSufficient ethyl acetate was added
4. dissolutionto dissolve the residue
5. washthe solution was washed with saturated aqueous sodium hydrogen carbonate
6. dry with materialbrine, dried (Na2SO4)
7. customevaporated in vacuo
8. customTrituration of the residue with dichloromethane gave a white solid, which
9. customwas removed by filtration
10. customEvaporation of the filtrate solution
11. customprovided a second crop of white solid
12. customThe evaporation-trituration procedure
13. customto give two further crops of white solid
14. washThe combined white solids were washed with ether
15. customdried in vacuo