反应详情

温度

100 °C

A mixture of ethyl (2E)-3-(5-chloro-2-pyrazinyl)acrylate (300 mg, 1.41 mmol), (3R)-1-(4-fluorobenzyl)-3-pyrrolidinamine dihydrochloride (565 mg, 2.11 mmol) and triethylamine (928 mg, 9.17 mmol) was stirred at 100° C. for 6 hrs. The reaction mixture was evaporated in vacuo and the residue was partitioned between water and EtOAc. The organic layer was separated, washed water and brine, dried over magnesium sulfate, and evaporated in vacuo. The residue was purified by silica gel column chromatography (35% EtOAc/hexane˜50% EtOAc/hexane) to give ethyl (2E)-3-(5-{[(3R)-1-(4-fluorobenzyl)-3-pyrrolidinyl]amino}-2-pyrazinyl)acrylate (245 mg, 47%) as an oil.

1. customThe reaction mixture was evaporated in vacuo
2. customthe residue was partitioned between water and EtOAc
3. customThe organic layer was separated
4. washwashed water and brine
5. dry with materialdried over magnesium sulfate
6. customevaporated in vacuo
7. customThe residue was purified by silica gel column chromatography (35% EtOAc/hexane˜50% EtOAc/hexane)