28721-09-7

4698-11-7

32315-10-9

28721-09-7

1. 32.67 g (0.11 mol) of triphosgene dissolved in 300 mL of toluene was slowly added dropwise over a period of 6 hours to a mixture of 66.9 g (0.3 mol) of 10-methoxy-5H-dibenzo[b,f]azepine and 34.92 g (0.34 mol) of triethylamine in 800 mL of toluene at a temperature of 10-15 °C. 2. After completion of the reaction ( complete disappearance of 10-methoxy-5H-dibenz[b,f]azepine was confirmed by TLC monitoring), 200 mL of 30% ammonia was slowly added with vigorous stirring for several hours at room temperature.3. After the reaction mixture was layered, the organic phase was separated, the toluene phase was washed with water, and the reaction mixture was subsequently evaporated to dryness under reduced pressure.4. 69.0 g (85% of the theoretical yield) was obtained of a purity greater than 95% of 10-methoxy-5H-dibenz[b,f]azepine. Methoxy-5H-dibenz[b,f]azepine-5-carboxamide.