反应详情

温度

130 °C

Compound 513 (36 mg, 0.09 mmol) was dissolved in acetonitrile (2 mL) in a reaction vial. 2-Chloro-N-methyl-acetamide (30 mg, 0.28 mmol), K2CO3 (38 mg, 0.28 mmol) were added. The reaction vial was flushed with argon, closed and then stirred at 130° C. for 45 min. in a microwave oven. The reaction mixture was poured into a mixture of EtOAc:H2O (1:1, 10 mL). The layers were separated and the aqueous phase was extracted with EtOAc (3×5 mL). The combined organic layers were dried (MgSO4), filtered, concentrated in vacuo and purified by continuously gradient flash chromatography using EtOAc/petroleum ether (40-60)(v:v=1:3 to 100:0) as the eluent, affording the title compound as a yellow oil. 13C NMR (CDCl3) δ 190.1, 168.2, 155.7 (d), 153.2 (d), 149.2, 136.6, 135.0, 134.5, 133.4, 131.2, 130.5, 128.7 (d), 128.1, 127.1, 125.3, 119.6 (d), 117.4 (d), 116.1 (d), 115.6, 112.4, 68.0, 25.8, 17.9

1. customThe reaction
2. customvial was flushed with argon
3. customclosed
4. additionThe reaction mixture was poured into a mixture of EtOAc:H2O (1:1, 10 mL)
5. customThe layers were separated
6. extractionthe aqueous phase was extracted with EtOAc (3×5 mL)
7. dry with materialThe combined organic layers were dried (MgSO4)
8. filtrationfiltered
9. concentrationconcentrated in vacuo
10. custompurified by continuously gradient flash chromatography