反应详情

tert-butyl 4-[8-[[(2S)-1-benzylpyrrolidin-2-yl]methyl-tert-butoxycarbonyl-sulfamoyl]-5,8-diazaspiro[2.5]octan-5-yl]pyrrolo[2,3-d]pyrimidine-7-carboxylate (Intermediate 48) (0.57 mmol) was dissolved in DCM (10 mL) and added TFA (1 mL). The reaction mixture was stirred at rt for 16 h, then added NaHCO3 (15 mL) and extracted with EtOAc (2×25 mL). The combined organic phases were dried over Na2SO4, filtered and concentrated in vacuo. The product was purified by flash chromatography on silica using EtOAc and MeOH in heptane as eluent.

1. extractionadded NaHCO3 (15 mL) and extracted with EtOAc (2×25 mL)
2. dry with materialThe combined organic phases were dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe product was purified by flash chromatography on silica