反应详情

To a solution of 6-(1,4-Diazabicyclo[3.2.2]nonan-4-yl)-2-(3-chlorophenyl)-3-methylquinazolin-4(3H)-one (400 mg, 1.013 mmol) (Example 2AL) in dichloromethane (12 mL) was added 3-chloroperbenzoic acid (250 mg, 1.013 mmol) and the reaction stirred at ambient temperature for 3 h. Sodium carbonate solution was added to neutralise the acid and the aqueous saturated with sodium chloride. The organic layer was separated off and chromatographed on 10 g silica, eluting with dichloromethane with 10% ammonia in methanol (1 M). To remove the remaining impurities the mixture was purified by acidic prep hplc, product passed through a carbonate on silica cartridge (2 g) to remove the acid to afford 4-(2-(3-chlorophenyl)-3-methyl-4-oxo-3,4-dihydroquinazolin-6-yl)-1,4-diazabicyclo[3.2.2]nonane 1-oxide (112 mg, 0.273 mmol).

1. customThe organic layer was separated off
2. customchromatographed on 10 g silica
3. washeluting with dichloromethane with 10% ammonia in methanol (1 M)
4. customTo remove the remaining impurities the mixture
5. customwas purified by acidic prep hplc, product
6. customto remove the acid