反应详情

温度

50 °C

To a solution of (3S)-N-(4-oxocyclohexyl)-1-phenylpiperidine-3-carboxamide (10 mg, 0.00003 mol, prepared as example 171) in concentrated aqueous HCl (0.5 mL), was added sodium azide (2.27 mg, 0.0000350 mol) in small portions over 3 minutes with slow agitation. The temperature was slowly increased to 50° C. The reaction temperature was maintained at 50° C. for 8.5 h and then poured into 50 g of crushed ice and water. The solution was basified with cold 50% NaOH and the resulting solution was extracted with EtOAc(×3). The EtOAc extracts were combined, dried over MgSO4, filtered and evaporated to yield the crude product, which was purified by prep-HPLC. LCMS: (M+H)+=316.2.

1. customover 3 minutes
2. temperatureThe reaction temperature was maintained at 50° C. for 8.5 h
3. extractionthe resulting solution was extracted with EtOAc(×3)
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. customevaporated