反应详情

5-Bromopyrazin-2-ol (1.209 g, 6.91 mmol) was dissolved in DMF (10.0 mL) and sodium hydride (60% in mineral, 530 mg, 13.25 mmol) was added. The reaction flask was put in a water bath and stirred under argon for 15 minutes, and then (2-bromoethoxy)(tert-butyl)dimethylsilane (1.69 mL, 7.93 mmol) was added as a solution in DMF (4.7 mL total volume), followed by a ˜0.5 mL rinse with DMF. The reaction was stirred under argon at room temperature for 2 days. It was then quenched with water (50 mL) and extracted with EtOAc (3×50 mL). The organic extracts were combined, washed with water (4×50 mL) and brine (50 mL), dried over sodium sulfate, filtered, and concentrated. The material was taken on crude to the next step.

1. customThe reaction flask was put in a water bath
2. washrinse with DMF
3. stirringThe reaction was stirred under argon at room temperature for 2 days
4. customIt was then quenched with water (50 mL)
5. extractionextracted with EtOAc (3×50 mL)
6. washwashed with water (4×50 mL) and brine (50 mL)
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. concentrationconcentrated