反应详情

温度

-20 °C

Ethyl chloroformate (25 ml) is added to a stirred mixture of the acid compound of step 10 above (0.7 g) in CHCl3 -Et3N (25 ml/0.7 g) chilled to -20° C. and stirring is continued for one hour. Aminoquinuclidine (2.8 g) and a saturated aqueous K2CO3 solution (7 ml) are added to the reaction mixture. Stirring is continued for 2 hours while slowly warning to RT. The mixture is diluted with CHCl3 and H2O, stirred for 5 minutes and the aqueous layer was separated. The organic layer is washed with H2O, dried (MgSO4) and evaporated affording a foamy solid which is converted to the dihydrochloride salt by dissolving in HCl-MeOH and evaporating the solvent. The desired product in the form of the dihydrochloride salt is a hygroscopic material is determined to be the correct material by NMR. M.P.=151°-153° C. Elemental Analysis: Calc'd C: 49.95, H 5.92, N 10.28; Found C: 50.58, H 6.20, N 9.98.

1. stirringStirring
2. waitis continued for 2 hours
3. customwhile slowly warning to RT
4. stirringstirred for 5 minutes
5. customthe aqueous layer was separated
6. washThe organic layer is washed with H2O
7. dry with materialdried (MgSO4)
8. customevaporated
9. customaffording a foamy solid which
10. customevaporating the solvent