反应详情

In a dried 100 mL round bottom flask was added cyclobutylamine (740 mg, 889 μL, 10.4 mmol, Eq: 3), K2CO3 (480 mg, 3.47 mmol, Eq: 1.00) and THF at rt. under argon. To the mixture was added a solution of (5-Bromomethyl-pyrazin-2-yl)-carbamic acid tert-butyl ester (1 g, 3.47 mmol, Eq: 1.00) in THF dropwise. The resulting reaction mixture was stirred vigorously at room temperature under argon overnight. The reaction was concentrated, diluted with water/DCM and extracted with DCM (2×30 mL). Combined organic extracts were concentrated to give a solid. The crude product was purified by LC chromatography (50 g spherical silica column) eluting with 5 to 10% MeOH in 1/1 EtOAc/Hex to afford 348 mg (36%) of the title compound as a white solid.

1. customThe resulting reaction mixture
2. concentrationThe reaction was concentrated
3. additiondiluted with water/DCM
4. extractionextracted with DCM (2×30 mL)
5. concentrationCombined organic extracts were concentrated
6. customto give a solid
7. customThe crude product was purified by LC chromatography (50 g spherical silica column)
8. washeluting with 5 to 10% MeOH in 1/1 EtOAc/Hex