反应详情

温度

0 °C

A 500 mL dry round bottom flask equipped with a magnetic stir bar was charged with 3,6-diethyl-N-(1-ethylpropyl)pyrazin-2-amine (10.0 g, 45.18 mmol) and CH2Cl2 (220 mL). After the mixture was cooled with an ice bath, N-bromosuccinimide (8.84 g, 49.7 mmol) was added at once. The mixture was stirred at 0° C. for 30 minutes then quenched with saturated aq. NaHCO3, diluted with H2O and extrated twice with CH2Cl2. The organics were combined, dried with NaSO4, filtered and concentrated to 13.96 g of a brown oil. The crude was purified by Biotage MPLC in two batches (120 g columns, 2.5% ethyl acetate in heptane.) Like fractions were combined to give 11.57 g (85%) of 5-bromo-3,6-diethyl-N-(1-ethylpropyl)pyrazin-2-amine as a yellow oil.

1. customA 500 mL dry round bottom flask
2. customequipped with a magnetic stir bar
3. temperatureAfter the mixture was cooled with an ice bath
4. customthen quenched with saturated aq. NaHCO3
5. additiondiluted with H2O
6. dry with materialdried with NaSO4
7. filtrationfiltered
8. concentrationconcentrated to 13.96 g of a brown oil
9. customThe crude was purified by Biotage MPLC in two batches (120 g columns, 2.5% ethyl acetate in heptane.) Like fractions