反应详情

A mixture of 15.0 parts of 1-(2-hydroxyethyl)-2-methyl-5-nitroimidazole tosylate and 7.5 parts of 2,4(1H,-3H)-quinazolinedione is dissolved in 190 parts of warm dimethylformamide. 2.9 Parts of potassium hydroxide is dissolved in 80 parts of methanol and diluted with about 95 parts of dimethylformamide. The methanol is removed under reduced pressure, the residual solution added to the quinazolinedione solution, and the resulting mixture heated on a steam bath for 4 hours. The crude solution is cooled, filtered, and diluted with 100 parts of water. The precipitate which forms is separated by filtration and the solvent is evaporated from the filtrate to leave a residue which is stirred with 630 parts of toluene and filtered. The solvent is evaporated from the filtrate to leave a yellow residue. This is dissolved in toluene and dimethylformamide and then concentrated. A precipitate forms and it is separated by filtration to give 3-[2-(2-methyl-5-nitro-1-imidazolyl)ethyl]-2,4-(1H,3H)quinazolinedione melting at about 261°-264° C.

1. customThe methanol is removed under reduced pressure
2. additionthe residual solution added to the quinazolinedione solution
3. temperaturethe resulting mixture heated on a steam bath for 4 hours
4. temperatureThe crude solution is cooled
5. filtrationfiltered
6. additiondiluted with 100 parts of water
7. customThe precipitate which forms is separated by filtration
8. customthe solvent is evaporated from the filtrate
9. customto leave a residue which
10. filtrationfiltered
11. customThe solvent is evaporated from the filtrate
12. customto leave a yellow residue
13. concentrationdimethylformamide and then concentrated
14. customA precipitate forms and it is separated by filtration