反应详情

To a mixture of 2.3 g of cyanogen bromide and 5.0 g of potassium carbonate in 40 ml of chloroform is added portion-wise over a 50 minutes span a solution of 4.8 of 2-fluoro-10,11-dihydro-11-[β-(dimethylamino)ethylthio]dibenz[b,f]oxepin, free base of Example 32, in 85 ml of chloroform. After total addition, the mixture is stirred for 20 minutes before being filtered. The filtrate is evaporated to leave an oil which is treated with three portions of boiling hexane. The combined hexane portions are evaporated leaving an oil which is chromatographed through a silica gel column with an eluant of methylene chloride and is recrystallized from cold hexane to give a white powder, mp 46°-48° C. of 11-[β-(bromo)ethylthio]-2-fluoro-10,11-dihydrodibenz[b,f]oxepin.

1. additionis added portion-wise over a 50 minutes
2. additionAfter total addition
3. filtrationbefore being filtered
4. customThe filtrate is evaporated
5. customto leave an oil which
6. customThe combined hexane portions are evaporated
7. customleaving an oil which
8. customis chromatographed through a silica gel column with an eluant of methylene chloride
9. customis recrystallized from cold hexane