反应详情

To a stirred slurry of 3.0 g (11 mmol) of the product from the previous step in 30 ml dry ether is added 5.5 ml of a 70% benzene solution of sodium bis-2-methoxyethoxyaluminum hydride at -20° C. under N2. The temperature of the mixture is raised to +10° C. for 20 minutes and the mixture is recooled to -20° C. and treated dropwise with 33 ml 4 N aqueous hydrochloric acid. The aqueous acid layer is extracted with chloroform, adjusted to pH8 with sodium bicarbonate and the crude title base extracted with chloroform and chromatographed on silica gel. Elution with ethylacetatechloroform gives fractions containing 0.8 g (29%) of pure title base which is converted to the hydrochloride, mp 254° C. dec in ethanol-isopropanol containing hydrochloric acid.

1. temperatureThe temperature of the mixture is raised to +10° C. for 20 minutes
2. customis recooled to -20° C.
3. extractionThe aqueous acid layer is extracted with chloroform
4. extractionthe crude title base extracted with chloroform
5. customchromatographed on silica gel
6. washElution with ethylacetatechloroform
7. customgives fractions