反应详情

step 6—To solution of 88 (0.087 g, 0.19 mmol) in DCM (5 mL) at 0° C. was added pyridine (23 □L) and followed by acetic anhydride (0.02 mL, 0.23 mmol). The reaction was allowed to warm to RT and stirred overnight then diluted with DCM and saturated aqueous NaHCO3. The aqueous layer was separated and extracted with DCM. The combined extract was washed with brine, dried (Na2SO4), filtered and concentrated. The crude product was purified on a preparative SiO2 TLC plate developed with 40% EtOAc/hexanes to afford 0.045 g (46%) of N-[4-tert-butyl-2-[2-(4-methanesulfonylamino-phenyl)-ethyl]-6-(2-methoxy-pyridin-3-yl)-phenyl]-acetamide (90) as an off-white solid.

1. customThe aqueous layer was separated
2. extractionextracted with DCM
3. extractionThe combined extract
4. washwas washed with brine
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated
8. customThe crude product was purified on a preparative SiO2 TLC plate