反应详情

To a solution of 3.0 g of 3-aminoquinuclidine and 3.0 g of N-methylmorpholine in 60 ml of chloroform is added 6.2 g of 6-chloro-3,4-dihydro-4-methyl-3-oxo-2H-1,4-benzoxazine-8-carboxylic acid chloride under cooling and stirring followed by stirring for 2 hours. The resultant solution is washed with water, aqueous sodium hydrogen carbonate and then water, and dried over magnesium sulfate. After the solvent is distilled off under reduced pressure, the residue is recrystallized from ethanol-isopropyl ether and treated with ethanolic hydrochloric acid to give 6-chloro-3,4-dihydro-4-methyl-3-oxo-N-(3-quinuclidinyl)-2H-1,4-benzoxazine-8-carboxamide hydrochloride, melting at 281° C. with decomposition.

1. temperatureunder cooling
2. stirringby stirring for 2 hours
3. washThe resultant solution is washed with water, aqueous sodium hydrogen carbonate
4. dry with materialwater, and dried over magnesium sulfate
5. distillationAfter the solvent is distilled off under reduced pressure
6. customthe residue is recrystallized from ethanol-isopropyl ether
7. additiontreated with ethanolic hydrochloric acid