反应详情

温度

20 °C

A charge of 26 kgs. toluene, 2.5 kgs. 2-methylmercaptoimidazoline hydroiodide, 2.4 kgs. N-(p-fluorobenzyl)isatoic anhydride and 1.55 kgs. powdered anhydrous sodium carbonate is refluxed for 18 - 20 hours in a reaction vessel which is vented to a caustic gas washing tower. Any water formed during the reaction is collected in a Dean-Stark separator. The reaction is cooled to 20°C. and 10 kgs. water added. The mixture is stirred for about 30 minutes and the solids collected, washed several times with 2 kg. portions of water, and three times with 0.8 kg. toluene. The solids are then dried at reduced pressure (about 55°C.) to obtain a crude product, m.p. 196°-198°C. The crude is dissolved at 50°C. in a solution of 14 kgs. chloroform and 4 kgs. ethanol and treated in solution with 0.1 kg. decoloring charcoal for about 10 minutes. The charcoal is removed by filtration through a celite bed and solids reprecipitated by concentrating the filtrate to a volume of about 8 liters. This concentrate is cooled to 0°-5°C., the solids collected by filtration, washed with cold ethanol and then diethyl ether, and dried at reduced pressure to obtain 10-(4'-fluorobenzyl)-2,3-dihydro-imidazo[2,1-b]quinazolin-5(10H)-one, m.p. 197°-198°C.

1. washwashing tower
2. customAny water formed during the reaction
3. customis collected in a Dean-Stark separator
4. additionwater added
5. customthe solids collected
6. washwashed several times with 2 kg
7. customThe solids are then dried at reduced pressure (about 55°C.)
8. customto obtain a crude product, m.p. 196°-198°C
9. customThe charcoal is removed by filtration through a celite bed and solids
10. customreprecipitated
11. concentrationby concentrating the filtrate to a volume of about 8 liters
12. temperatureThis concentrate is cooled to 0°-5°C.
13. filtrationthe solids collected by filtration
14. washwashed with cold ethanol
15. dry with materialdiethyl ether, and dried at reduced pressure