反应详情

温度

0 °C

20 g (85 mmols) of (I) are dissolved in 120 ml of CH2Cl2. The solution is cooled to 0° C. and added with 0.24 g of 2,2,6,6-tetramethylpiperidine nitroxide, then with 180 ml of 1.4M NaClO, adjusted to pH 8.3 with a NaHSO4 saturated solution. The mixture is left for 1 hour at 0° C., then warmed to 20° C. for 4 hours. The organic phase is separated and washed with 50 ml of water, dried with 2 g of Na2SO4 and solvent is evaporated off. The residue is taken up with 50 ml of acetone and kept at 0° C. for 2 hours. The mixture is filtered, washed with 50 ml of cold acetone, dried at 60° C. for 4 hours to obtain 17 g of 5-cyano-10-oxo-10,11-dihydro-5H-dibenz[b,f]azepine (VII), m.p. 153-4° C., with 98.5% purity by HPLC (85% yield).

1. temperaturewarmed to 20° C. for 4 hours
2. customThe organic phase is separated
3. washwashed with 50 ml of water
4. dry with materialdried with 2 g of Na2SO4 and solvent
5. customis evaporated off
6. waitkept at 0° C. for 2 hours
7. filtrationThe mixture is filtered
8. washwashed with 50 ml of cold acetone
9. customdried at 60° C. for 4 hours