反应详情

To a mixture of the 4-chloro-thionicotinamide (5.5 g, 31.9 mmol) and EtOH (300 mL) was added bromo-ethyl-pyruvate (4.4 mL, 35.1 mmol). The mixture was heated at reflux for 15 h, cooled and concentrated in vacuo to afford a yellow solid/orange oil. The oil was diluted with EtOAc and filtered off yellow solid. The filtrate was filtered through Celite® and concentrated in vacuo to give a dark yellow oil. The oil was diluted with 2% MeOH/CH2Cl2 and filtered through a pad of silica gel (150 mL). Elution with 2% MeOH/CH2Cl2 (500 mL), followed by concentration in vacuo afforded the title compound as a yellow crystalline solid. MS m/z: 269.1 (M+H).

1. temperatureThe mixture was heated
2. temperatureat reflux for 15 h
3. temperaturecooled
4. concentrationconcentrated in vacuo
5. customto afford a yellow solid/orange oil
6. filtrationfiltered off yellow solid
7. filtrationThe filtrate was filtered through Celite®
8. concentrationconcentrated in vacuo
9. customto give a dark yellow oil
10. filtrationfiltered through a pad of silica gel (150 mL)
11. washElution with 2% MeOH/CH2Cl2 (500 mL)
12. concentrationfollowed by concentration in vacuo