反应详情

温度

90 °C

A mixture of 1-((2-(dimethoxymethyl)-5,6,7,8-tetrahydro-1,8-naphthyridin-3-yl)methyl)-4-methylpiperazin-2-one (intermediate 81, 1.03 g, 3.08 mmol), phenyl(5-cyano-4-(2-methoxyethoxyl)pyridin-2-yl)carbamate (intermediate 108, 2.19 g, 6.16 mmol) and DMAP (753 mg, 6.16 mmol) in DMA (15 ml) was heated at 90° C. for 3.5 h. The cooled reaction mixture was partitioned between EtOAc and, the organic layer dried over MgSO4 and evaporated. The residue was purified by reversed phase chromatography (RP 4) and the product containing fractions were partitioned between saturated aqueous NaHCO3 and EtOAc, the organic layer dried over MgSO4 and vaporated. The residue was then triturated with a mixture of DCM, Et2O and heptane to give the title compound as a white solid. (UPLC-MS 7) tR 0.80; ESI-MS 554.4 [M+H]+.

1. customThe cooled reaction mixture
2. customwas partitioned between EtOAc
3. dry with materialthe organic layer dried over MgSO4
4. customevaporated
5. customThe residue was purified by reversed phase chromatography (RP 4)
6. additionthe product containing fractions
7. customwere partitioned between saturated aqueous NaHCO3 and EtOAc
8. dry with materialthe organic layer dried over MgSO4
9. customThe residue was then triturated with a mixture of DCM, Et2O and heptane