反应详情

温度

80 °C

To a solution of ethyl 3-methyl-1H-pyrrole-4-carboxylate (3.15 g, 20.5 mmol) in acetonitrile (MeCN) were added potassium carbonate (5.7 g, 41 mmol) and 2,4-dichloro-5-fluoropyrimidine (3.4 g, 20.5 mmol) at room temperature. The resulting slurry was heated at 80° C. for 3 hours with monitoring a reaction with LC-MS or thin layer chromatography (TLC). It was diluted with ethyl acetate and washed with brine. The collected organic layer was dried over anhydrous sodium sulfate and then partially concentrated in vacuo. To this, n-hexanes were added to form pale yellow precipitates. The resulting solids were collected by filtration and rinsed with n-hexanes and then dried under high vacuum to give 4.9 g (85%) of the target intermediate 3; MS (ESI) m/z 285 [M+H]+

1. customa reaction with LC-MS or thin layer chromatography (TLC)
2. washwashed with brine
3. dry with materialThe collected organic layer was dried over anhydrous sodium sulfate
4. concentrationpartially concentrated in vacuo
5. additionTo this, n-hexanes were added
6. customto form pale yellow precipitates
7. filtrationThe resulting solids were collected by filtration
8. washrinsed with n-hexanes
9. customdried under high vacuum