反应详情

Tritylamine (180 mg, 0.00068 mol) was added to a solution of 1-tert-butyl 3-ethyl 3-(2-oxoethyl)piperidine-1,3-dicarboxylate (0.170 g, 0.000568 mol, this was prepared by using procedures analogous to that described for the synthesis of example 1, steps 1-2) in 1,2-dichloroethane (4.0 mL, 0.051 mol) and followed by sodium triacetoxyborohydride (0.36 g, 0.0017 mol) and the mixture was stirred overnight. The mixture was poured into pre-cooled water, and extracted with ethyl acetate. The organic layer was separated, dried (NaSO4), and concentrated in-vacuo. The product was purified by CombiFlash eluting with hexane/EtOAc (max EtOAc 20%). LC-MS: 543.3 (M+H)+; 243.2.

1. customthis was prepared
2. additionThe mixture was poured
3. extractionextracted with ethyl acetate
4. customThe organic layer was separated
5. dry with materialdried (NaSO4)
6. concentrationconcentrated in-vacuo
7. customThe product was purified by CombiFlash
8. washeluting with hexane/EtOAc (max EtOAc 20%)