反应详情

5-Bromonicotinic acid (1 g, 4.950 mmol) is placed in a 100 ml round bottomed flask and purged with Argon. Dry THF (20 ml) is added and the resulting solution is treated with NaH (60% dispersed in mineral oil) (0.202 g, 5.049 mmol) over a period of 5 minutes. The reaction mixture is stirred at room temperature for 10 minutes and then oxalyl chloride (0.453 ml, 5.198 mmol) is added slowly over 5 minutes followed by dry DMF (10 ul). The reaction mixture is stirred for a further 5 minutes, filtered through filter paper, concentrated in vacuo and dried under vacuum to afford the title compound.

1. custompurged with Argon
2. additionDry THF (20 ml) is added
3. stirringThe reaction mixture is stirred for a further 5 minutes
4. filtrationfiltered
5. filtrationthrough filter paper
6. concentrationconcentrated in vacuo
7. customdried under vacuum