反应详情

(R)-Quinuclidin-3-yl 2-amino-2-phenylacetate dihydrochloride (C25) (1.11 g, 3.33 mmol) is dissolved in MeOH (10 mL) and 32% NH4OH (2.0 mL, 16.07 mmol) is added. The solution is stirred at RT for 30 seconds and then is evaporated under vacuum. The residue is dissolved in DCM/MeOH (4.5/0.5 mL) and about 1 g of SiO2 is added. The suspension is evaporated and the residue is loaded on a silica gel column and purified eluting with DCM/MeOH/NH4OH=9.2/0.8/0.1 to 9/1/0.1 to collect intermediate I124 as a pale yellow oil (635 mg, 73% yield).

1. customis evaporated under vacuum
2. dissolutionThe residue is dissolved in DCM/MeOH (4.5/0.5 mL)
3. additionabout 1 g of SiO2 is added
4. customThe suspension is evaporated
5. custompurified
6. washeluting with DCM/MeOH/NH4OH=9.2/0.8/0.1 to 9/1/0.1