反应详情

温度

40 °C

A mixture of 100 gms of 10-methoxyiminostilbene in 1000 mL of toluene containing 106 gms of monochloro-acetic acid and 73 gms of sodium cyanate were heated to 40° C. under stirring and maintained for 4 hours. After completion of the reaction (monitored by HPLC and/or TLC), the mixture was cooled to room temperature, filtered and washed with 5% sodium carbonate solution followed by water. The toluene layer was then added to 1000 mL of 2N hydrochloric acid, and the mixture was heated to 75-80° C. and maintained for 2 hours under good agitation. It was then cooled to 0-5° C. and maintained for 2 hours, and the product oxcarbazepine was separated by filtration. This was then purified twice in toluene:methanol followed by methanol:dichloromethane solvent mixture to furnish 28 gms of pure oxcarbazepine.

1. temperaturemaintained for 4 hours
2. customAfter completion of the reaction (monitored by HPLC and/or TLC)
3. temperaturethe mixture was cooled to room temperature
4. filtrationfiltered
5. washwashed with 5% sodium carbonate solution
6. additionThe toluene layer was then added to 1000 mL of 2N hydrochloric acid
7. temperaturethe mixture was heated to 75-80° C.
8. temperaturemaintained for 2 hours under good agitation
9. temperatureIt was then cooled to 0-5° C.
10. temperaturemaintained for 2 hours
11. customthe product oxcarbazepine was separated by filtration
12. customThis was then purified twice in toluene