反应详情

A mixture of ethyl 5-amino-6-bromopyrazine-2-carboxylate (210 mg, 0.853 mmol), tert-butyl 2-fluoro-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoate (357 mg, 1.109 mmol), PdCl2(dppf).CH2Cl2 adduct (69.7 mg, 0.085 mmol) and Na2CO3 (362 mg, 3.41 mmol) (2M solution was used) in DME (5 mL) was placed into a 20 ml vial and sealed. The mixture was microwaved for 15 min at 110° C. The mixture was diluted with EtOAc, washed with water twice and brine, dried, filtered, and concentrated to afford the crude as a light yellow solid. The crude product was purified by ISCO (12 g, 10-55% EtOAc in heptane, 30 min) to afford 228 mg (74% yield) of light yellow solid. LC-MS (m/z): 362.1 (MH+), 0.89 min.

1. customsealed
2. customThe mixture was microwaved for 15 min at 110° C
3. washwashed with water twice
4. dry with materialbrine, dried
5. filtrationfiltered
6. concentrationconcentrated
7. customto afford the crude as a light yellow solid
8. customThe crude product was purified by ISCO (12 g, 10-55% EtOAc in heptane, 30 min)
9. customto afford 228 mg (74% yield) of light yellow solid
10. custom362.1 (MH+), 0.89 min.