反应详情

温度

70 °C

A mixture of 2-(trimethylsilyl)ethyl 4-((8-((5-cyano-4-((2-methoxyethyl)amino)pyridin-2-yl)carbamoyl)-2-(dimethoxymethyl)-5,6,7,8-tetrahydro-1,8-naphthyridin-3-yl)methyl)-3-oxopiperazine-1-carboxylate (intermediate 122, 4.20 g, 5.29 mmol) and tetraethylammonium fluoride dihydrate (2.53 g, 13.22 mmol) in AcCN (50 ml) was heated for 30 minutes at 70° C. The reaction mixture was partitioned between saturated aqueous NaHCO3 solution and DCM, the DCM phase washed with brine, dried over MgSO4 and evaporated. The residue was applied to a RediSep® silica column and purified by normal phase chromatography, eluting with EtOAc then a gradient from DCM to 10% MeOH in DCM. Product containing fractions were combined and evaporated to give the title compound as a yellow-white solid. (UPLC-MS 7) tR 0.68; ESI-MS 539.5 [M+H]+.

1. customThe reaction mixture was partitioned between saturated aqueous NaHCO3 solution and DCM
2. washthe DCM phase washed with brine
3. dry with materialdried over MgSO4
4. customevaporated
5. custompurified by normal phase chromatography
6. washeluting with EtOAc
7. additionProduct containing fractions
8. customevaporated