反应详情

A mixture of 5-bromopyrazin-2-amine (1.2 g, 6.9 mmol) and pyrrolidine (4 mL, 48 mmol) was microwaved at 180° C., 200 W for 2 h. The reaction was diluted into 125 mL ethyl acetate and extracted with water (3×50 mL) and brine (50 mL). It was dried over sodium sulfate, filtered and concentrated. The crude product was purified by column chromatography (0 to 3% methanol/methylene chloride) to afford 5-(pyrrolidin-1-yl)pyrazin-2-amine (495 mg, 3. mmol, 43.7% yield). 1H NMR (400 MHz, DMSO-d6) δ ppm 7.52 (1H, d, J=1.51 Hz), 7.36 (1H, d, J=1.76 Hz), 5.21 (2H, s), 3.24-3.29 (4H, m), 1.90 (4H, ddd, J=6.48, 3.53, 3.34 Hz). MS (LC/MS) R.T.=0.52; [M+H]+=165.29.

1. customwas microwaved at 180° C.
2. extractionextracted with water (3×50 mL) and brine (50 mL)
3. dry with materialIt was dried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customThe crude product was purified by column chromatography (0 to 3% methanol/methylene chloride)