反应详情

To a solution of 9-benzyl-9-azabicyclo[3.3.1]nonan-3-one (0.5 g) in chloroform (4.4 ml), cooled down to −5° C., 1 ml of conc. H2SO4 is dropwise added while maintaining the temperature below 15° C. Then NaN3 (0.28 g) is slowly added, at small portions so to avoid temperatures in the reaction mixture higher than 35° C. The mixture is then heated at reflux for 2 hours. The reaction mixture is poured into a vessel containing about 200 ml of ice. Solid K2CO3 is added up to a strongly alkaline pH. An emulsion is formed, that is added of 25 ml of a 60% KOH aqueous solution. Stirring is effected for 10 minutes. At the end the formed inorganic salts are filtered and the reaction mixture extracted with chloroform. The organic phase is dehydrated with sodium sulphate and the solvent evaporated. 0.50 g of 10-benzyl-3,10-diazabicyclo[4.3.1]decan-4-one (1py1) are obtained as a light solid.

1. temperaturewhile maintaining the temperature below 15° C
2. customhigher than 35° C
3. temperatureThe mixture is then heated
4. temperatureat reflux for 2 hours
5. additionThe reaction mixture is poured into a vessel
6. customAn emulsion is formed
7. filtrationAt the end the formed inorganic salts are filtered
8. extractionthe reaction mixture extracted with chloroform
9. customthe solvent evaporated