反应详情

温度

-10 °C

4.47 g of the product obtained in Stage 1 above, 11.2 ml of triglyme, 2.78 g of 5,5-dimethyl hydantoin and 1.34 g of cuprous oxide are introduced then the suspension is agitated and taken to 215° C. for 4 hours. Then it is returned to ambient temperature, followed by filtering, washing with 4.5 ml of triglyme and agitating without exceeding 25° C., 4.5 ml of 22°Be concentrated ammonium hydroxide, 26 ml of water and 4.5 ml of toluene. Agitation is carried out for 15 minutes at 20° C. then the reaction medium is cooled down to -10° C., agitation is carried out for 1 hour, followed by separating, washing with 2.2 ml of toluene then 4.5 ml of water and drying. In this way 1.98 g of expected product (brown crystals) is obtained. M.p.=210° C.

1. customis returned to ambient temperature
2. filtrationby filtering
3. washwashing with 4.5 ml of triglyme
4. stirringagitating
5. customwithout exceeding 25° C.
6. waitAgitation is carried out for 15 minutes at 20° C.
7. waitagitation is carried out for 1 hour
8. customby separating
9. washwashing with 2.2 ml of toluene
10. dry with material4.5 ml of water and drying