反应详情

1-(3-Fluoro-2-methylquinoxalin-5-yl)ethanone (126g, 2.00 g, 9.79 mmol) was treated with HCl (4.0 M solution in 1,4-dioxane; 24.49 ml, 98 mmol), and the homogeneous reaction was fitted with a drying tube. After 6 h the reaction was concentrated in vacuo, and the solid was taken up in DCM. Solid NaHCO3 was added cautiously with rapid stirring; and saturated aq. NaHCO3 was sequentially added cautiously with rapid stirring. The mixture was partitioned between saturated NaHCO3 and DCM. The aq. layer was extracted with DCM (2×), and the combined organics were dried over anhydrous Na2SO4, filtered, and concentrated in vacuo to give 1-(3-chloro-2-methylquinoxalin-5-yl)ethanone (254a, 99% yield) as an orange-brown solid. MS (ESI, pos. ion) m/z: 221.0 (M+1).

1. customthe homogeneous reaction
2. customwas fitted with a drying tube
3. concentrationAfter 6 h the reaction was concentrated in vacuo
4. additionSolid NaHCO3 was added cautiously with rapid stirring
5. additionand saturated aq. NaHCO3 was sequentially added cautiously with rapid stirring
6. customThe mixture was partitioned between saturated NaHCO3 and DCM
7. extractionThe aq. layer was extracted with DCM (2×)
8. dry with materialthe combined organics were dried over anhydrous Na2SO4
9. filtrationfiltered
10. concentrationconcentrated in vacuo