反应详情

温度

140 °C

A mixture of 2-bromo-N-(3-(quinoxalin-2-yl)phenyl)acetamide (300 mg, 0.876 mmol) and potassium thioacetate (400 mg, 3.5 mmol) in acetonitrile (15 mL) was heated in microwave at 140° C. for 10 min. The dark red solution was diluted with ethylacetate (50 mL), washed with brine (2×50 mL), dried over sodium sulphate, the solvent was evaporated in vacuo and the residue was purified by flash column chromatography (Flash Master, 20 g Isolute Silica column, gradient 0 to 5 min hexane, then ethyl acetate up to 50% over 20 min) to afford S-2-oxo-2-(3-(quinoxalin-2-yl)phenylamino)ethyl ethanethioate (40 mg, 13% yield). LCMS calculated for C18H15N3O2S (M+H): 338.40. found 338. 1H-NMR (DMSO-d6, 400 Mhz) δH: 10.45 (1H, br.), 9.50 (1H, s), 8.51 (1H, m), 8.11-8.18 (2H, m), 8.05-8.08 (1H, m), 7.80-7.95 (3H, m), 7.55-7.60 (1H, m), 3.90 (2H, s), 2.41 (3H, s).

1. washwashed with brine (2×50 mL)
2. dry with materialdried over sodium sulphate
3. customthe solvent was evaporated in vacuo
4. customthe residue was purified by flash column chromatography (Flash Master, 20 g Isolute Silica column, gradient 0 to 5 min hexane