反应详情

To a solution of tert-butyl 8-(2-(6-(((tert-butyldimethylsilyl)oxy)methyl)-7-(dimethoxymethyl)-1,2,3,4-tetrahydro-1,8-naphthyridine-1-carboxamido)-5-cyanopyridin-4-yl)-2,8-diazaspiro[4.5]decane-2-carboxylate (intermediate 37D, 70 mg, 0.095 mmol) in THF (0.5 ml) and H2O (0.5 ml) was added conc. HCl (0.1 ml, 1.2 mmol). The reaction mixture was stirred at room temperature for 4 h, then conc. HCl (0.1 ml, 1.2 mmol) was added and the reaction mixture was stirred at room temperature overnight. The reaction mixture was poured into sat. aq. NaHCO3 and extracted with DCM (4×) and EtOAc (4×). The combined organic phases were then dried over Na2SO4, filtered and evaporated. The crude material was triturated with EtOAc and dried under high vacuum to give the title compound as an off-white powder. (UPLC-MS 3) tR 0.64 min; ESI-MS 476.2 [M+H]+.

1. stirringthe reaction mixture was stirred at room temperature overnight
2. extractionextracted with DCM (4×) and EtOAc (4×)
3. dry with materialThe combined organic phases were then dried over Na2SO4
4. filtrationfiltered
5. customevaporated
6. customThe crude material was triturated with EtOAc
7. customdried under high vacuum