反应详情

To a solution of 10 g (105 mmol) of 2-aminopyrazine in 100 mL of pyridine was added dropwise a solution of 10.99 g (9.56 mL, 105 mmol) of cyclopropanecarbonyl chloride in 100 mL of dichloromethane. The resultant yellow solution was stirred at ambient temperature for 2 h. The reaction mixture was concentrated in vacuo. The residue was dissolved in ethyl acetate and a small amount of water and washed sequentially with 1 M aqueous cuprous sulfate solution and water. The water layer was extracted with three portions of ethyl acetate. The combined organic phases were washed with brine, dried over magnesium sulfate, and concentrated. Purification by flash chromatography (silica gel, eluting sequentially with 50%, 80% and 100% ethyl acetate/hexane) gave the title compound.

1. concentrationThe reaction mixture was concentrated in vacuo
2. dissolutionThe residue was dissolved in ethyl acetate
3. washa small amount of water and washed sequentially with 1 M aqueous cuprous sulfate solution and water
4. extractionThe water layer was extracted with three portions of ethyl acetate
5. washThe combined organic phases were washed with brine
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated
8. customPurification by flash chromatography (silica gel
9. washeluting sequentially with 50%, 80% and 100% ethyl acetate/hexane)