反应详情

A suspension of 6-iodo-2-trichloromethyl-1,2-dihydro-quinazolin-4-one (38.9 g=100 mmol) in POCl3 (500 mL) was heated to reflux for 12 hours. The homogeneous solution was cooled and excess POCl3 was distilled under vacuum. Viscous oil obtained was poured over crushed ice and triturated vigorously to give grey solid, which was dissolved in toluene (200 mL), filtered and evaporated under vacuo to give off-white crystalline solid. Mp 154°-155° C. Elemental Analysis: Calculated for C9H3Cl4IN2, C: 26.50, H, 0.74, N: 6.87; Found: C: 26.15, H: 0.79, N. 6.68.

1. temperaturewas heated
2. temperatureto reflux for 12 hours
3. temperatureThe homogeneous solution was cooled
4. distillationexcess POCl3 was distilled under vacuum
5. customViscous oil obtained
6. additionwas poured
7. customover crushed ice
8. customtriturated vigorously
9. customto give grey solid, which
10. filtrationfiltered
11. customevaporated under vacuo
12. customto give off-white crystalline solid