反应详情

To a solution of methyl 5-bromopyrazine-2-carboxylate (0.250 g, 1.152 mmol) in Tetrahydrofuran (THF) (6.53 ml) at 0° C. under nitrogen was added methylmagnesium bromide, 3 M in diethyl ether (1.152 ml, 3.46 mmol) slowly. After 1 hour at 0° C., 2N HCl (15 mL) was added slowly. The mixture was extracted with ethyl acetate (2×15 mL). The combined organic extracts were dried (Na2SO4), filtered, and concentrated. The residue was purified using silica gel chromatography CISCO): 10-30% ethyl acetate/hexanes (20 min), 12 gram silica gel column. Obtained 2-(5-bromopyrazin-2-yl)propan-2-ol as an orange oil (71 mg, 24%). MS (m/z) 216.9 (M+).

1. extractionThe mixture was extracted with ethyl acetate (2×15 mL)
2. dry with materialThe combined organic extracts were dried (Na2SO4)
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue was purified
6. custom10-30% ethyl acetate/hexanes (20 min), 12 gram silica gel column