反应详情

温度

77 °C

To a solution of methyl N-(3-ethoxy-3-oxopropanoyl)-N-(1-piperidinyl)-β-alaninate (43 g, 143 mmol) in a mixture of THF (2.26 L) and DMF (1.00 L) was added Cs2CO3 (140 g, 430 mmol). The resulting mixture was heated at reflux (77° C.) for 48 h. The cooled reaction was filtered, and the filtrate was evaporated. The filtrate residue and filtered solid were combined and purified by flash chromatography using 7:3 CH2Cl2/MeOH as eluant, to give 11.36 g of partially pure title material. LC-MS m/z 269.19 (MH+), retention time 2.20 min (method 2).

1. temperatureThe resulting mixture was heated
2. customThe cooled reaction
3. filtrationwas filtered
4. customthe filtrate was evaporated
5. filtrationThe filtrate residue and filtered solid
6. custompurified by flash chromatography
7. customto give 11.36 g of partially pure title material