反应详情

温度

120 °C

To a solution of methyl (2E)-3-(5-chloro-2-pyrazinyl)acrylate (680 mg) in DMI (1.4 mL) was added tert-butyl (3R)-3-amino-1-pyrrolidinecarboxylate (957 mg) and K2CO3 (1.42 g), which was stirred at 120° C. for 2 hours. The reaction mixture was filtered and evaporated in vacuo. To the residue was added H2O, which was extracted with ethyl acetate. The organic layer was washed with brine, dried over Na2SO4, filtered, and evaporated in vacuo. The residue was purified by column chromatography on silica gel to give tert-butyl (3R)-3-({5-[(1E)-3-methoxy-3-oxo-1-propen-1-yl]-2-pyrazinyl}amino)-1-pyrrolidinecarboxylate (834 mg) as a off-white powder.

1. filtrationThe reaction mixture was filtered
2. customevaporated in vacuo
3. additionTo the residue was added H2O, which
4. extractionwas extracted with ethyl acetate
5. washThe organic layer was washed with brine
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. customevaporated in vacuo
9. customThe residue was purified by column chromatography on silica gel