反应详情

20.45 g (0.09 mol) 6-(1-Aminopropyl)-3-phenyl-1,2,4-triazin-5(4H)-one (Example 34A) are dissolved in dichloroethane, 502 g (5.08 mol) triethylamine and 19.8 g (0.10 mol) cis-4-tert-butylcyclohexanecarbonyl chloride are added. The solution is stirred at reflux for three hours, then 20.42 g (0.13 mol) phosphoroxychloride are added. The solution is stirred at reflux for another 4 hours and, after cooling down to room temperature, water, sodium hydroxide and then dichloromethane are added. The organic phase is evaporated to dryness in vacuo, and the residue triturated with diethylether and filtrated. The solid is dissolved in methanol (75%)/dichloromethane (25%), the dichloromethane is evaporated in vacuo, and the crystallized product is filtered and dried.

1. temperatureat reflux for three hours
2. stirringThe solution is stirred
3. temperatureat reflux for another 4 hours
4. customThe organic phase is evaporated to dryness in vacuo
5. customthe residue triturated with diethylether
6. filtrationfiltrated
7. dissolutionThe solid is dissolved in methanol (75%)/dichloromethane (25%)
8. customthe dichloromethane is evaporated in vacuo
9. filtrationthe crystallized product is filtered
10. customdried