反应详情

To the resulting suspension is added dropwise with stirring, a solution of 3.33 g. (0.01 mol) 8-[3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]propyl]-8-azabicyclo[3.2.1]octan-3-one in 50 ml. dry tetrahydrofuran over 20 minutes while the reaction temperature is maintained between -65° C. to -75° C. The cold reaction mixture is then permitted to stir for 11/2 hours, then allowed to warm to room temperature, after which it is placed in an oil bath at +60° to 65° for 4 hours. After standing for about 16 hours, 50 ml. of water and 100 ml. of diethyl ether is added and following agitation the layers are partitioned. The aqueous solution is extracted two additional times with diethyl ether and all ethereal extracts are combined, dried over anhydrous sodium sulfate and concentrated to afford a viscous oil. The oil is dissolved in 300 ml. of acetone, 20 ml. of 1.2 N hydrochloric acid is added and the solution stirred for 4 hours. The solution is concentrated in vacuo, 100 ml. of 3 N hydrochloric acid is added and the solution is extracted with 150 ml. of diethyl ether. The hydrochloric acid solution is made basic with 15% sodium hydroxide aqueous solution, then extracted three times with 100 ml. portions of diethyl ether.

1. additionTo the resulting suspension is added dropwise
2. customThe cold reaction mixture
3. stirringto stir for 11/2 hours
4. waitAfter standing for about 16 hours
5. customare partitioned
6. extractionThe aqueous solution is extracted two additional times with diethyl ether
7. dry with materialdried over anhydrous sodium sulfate
8. concentrationconcentrated
9. customto afford a viscous oil
10. dissolutionThe oil is dissolved in 300 ml
11. stirringthe solution stirred for 4 hours
12. concentrationThe solution is concentrated in vacuo, 100 ml
13. additionof 3 N hydrochloric acid is added
14. extractionthe solution is extracted with 150 ml
15. extractionextracted three times with 100 ml