反应详情

To a solution of 1.78 g (47.0 mmol) of sodium borohydride in 100 ml of methanol, containing 10 ml of 6N sodium hydroxide, is added dropwise with stirring a solution of 3.20 g (9.41 mmol) of 2-amino-5,6-dihydro-7-methylpyrido[2,3-h]quinazolinium iodide, in 200 ml of a mixture of methanol and water (1:1). The solution is stirred at room temperature for 2 hours, cooled, acidified by dropwise addition of 10% hydrochloric acid and stirred at room temperature for 2 hours. The solution is concentrated, basified with concentrated ammonium hydroxide and extracted with chloroform. The chloroform extract is dried over magnesium sulfate, filtered and concentrated to a brown oil. Medium pressure chromatography (silica gel, 2% ammonium hydroxide--2% methanol--96% ethyl acetate) affords 0.45 g (22.2%) of the title compound as an orange solid; mp 204°-213° C.

1. additionis added dropwise
2. temperaturecooled
3. stirringstirred at room temperature for 2 hours
4. concentrationThe solution is concentrated
5. extractionextracted with chloroform
6. extractionThe chloroform extract
7. dry with materialis dried over magnesium sulfate
8. filtrationfiltered
9. concentrationconcentrated to a brown oil