反应详情

温度

27.5 °C

6,7-Bis(2-methoxy-ethoxy)-quinazolone (68 gm), chloroform (1360 ml) and dimethylformamide (7.5 ml) are taken in a reaction flask at 25-30° C. and stirring begun. To the contents is added oxalyl chloride (120 ml) at 25-30° C. slowly for 30 minutes, which is then heated to reflux for 1 hour 30 minutes. The solvent is distilled at 55-60° C. under vacuum, diisopropyl ether (560 ml) is added, cooled to 25-30° C. and then stirred for 30 minutes. The compound is filtered and washed with diisopropyl ether (100 ml). The compound is added to chloroform (1000 ml), the chloroform is washed two times with 8% NaHCO3 solution (each time 680 ml) and the resulting organic layer is washed with water (500 ml), the organic layer is dried over sodium sulfate and the solvent is distilled under a vacuum at 55-60° C. To the residue is added n-heptane and stirred for 1 hour at 25-30° C. The material, is filtered washed with n-heptane (100 ml) and then the material is dried at 50° C. under vacuum to obtain 65 gm of 4-Chloro-6,7-bis-(2-methoxyethoxy)-quinazoline.

1. temperaturewhich is then heated
2. temperatureto reflux for 1 hour 30 minutes
3. distillationThe solvent is distilled at 55-60° C. under vacuum, diisopropyl ether (560 ml)
4. additionis added
5. stirringstirred for 30 minutes
6. filtrationThe compound is filtered
7. washwashed with diisopropyl ether (100 ml)
8. additionThe compound is added to chloroform (1000 ml)
9. washthe chloroform is washed two times with 8% NaHCO3 solution (each time 680 ml) and the resulting organic layer
10. washis washed with water (500 ml)
11. dry with materialthe organic layer is dried over sodium sulfate
12. distillationthe solvent is distilled under a vacuum at 55-60° C
13. additionTo the residue is added n-heptane
14. stirringstirred for 1 hour at 25-30° C
15. filtrationThe material, is filtered
16. washwashed with n-heptane (100 ml)
17. customthe material is dried at 50° C. under vacuum