反应详情

温度

80 °C

To a solution of tert-butyl (3R,4S)-3-({cyclopropyl[3-hydroxy-5-(3-methoxy-propyl)benzyl]amino}carbonyl)-4-{4-[2-(2,6-dichloro-4-methylphenoxy)ethoxy]-phenyl}piperidine-1-carboxylate (1 eq.) from Example 1/Step 2 in DMF was added potassium carbonate (4.4 eq.) and 2-chloro-N,N-dimethylethanamine hydrochloride (2.5 eq.). The reaction was heated to 80° C. and stirred for 4 hr. After cooling to rt, the reaction was diluted with ether. The organic extract was washed with 5% aqueous potassium carbonate solution, brine, dried over MgSO4, and concentrated in vacuo. The crude product was purified by flash column chromatography (SiO2, 2%→5% [2 M NH3 in MeOH] in DCM) to afford the title compound as an oil.

1. temperatureAfter cooling to rt
2. extractionThe organic extract
3. washwas washed with 5% aqueous potassium carbonate solution, brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. customThe crude product was purified by flash column chromatography (SiO2, 2%→5% [2 M NH3 in MeOH] in DCM)