反应详情

温度

2.5 °C

50 ml of CH2Cl2 and 5 g (0.0227 mols) of (I) are loaded into a 250 ml pyrex round-bottom flask, under nitrogen and stirring, then 2.4 g of Na2CO3 (0.045 mols) are added thereto. The mixture is cooled to 0-5° C., irradiated from the outside with a 300 watt halogen lamp while adding a 1:1 chlorine and nitrogen gaseous mixture with 6 ml/minute flow, for 3 hours, then nitrogen for 10 minutes at the same flow rate. The mixture is filtered at 30° C. and methylene chloride is evaporated off. The residue is taken up with 15 ml of hexane and 4 ml of ethyl acetate, refluxed for 15 minutes, then cooled to 0° C. for 2 hours. The solid residue is recrystallized twice with the same solvent, to obtain 2.5 g (43% yield) of 5-cyano-10-chloro-10,11-dihydro-5H-dibenz[b,f]azepine (III) with melting point 139-140° C.

1. waitnitrogen for 10 minutes at the same flow rate
2. filtrationThe mixture is filtered at 30° C.
3. custommethylene chloride is evaporated off
4. temperaturerefluxed for 15 minutes
5. temperaturecooled to 0° C. for 2 hours
6. customThe solid residue is recrystallized twice with the same solvent