反应详情

To a suspension of 5-methyl-nicotinamide from step 2 (10.5 g, 0.077 mmol) in triethylamine (23.3 g, 0.23 mmol) and 400 mL of methylene chloride was added trifluoroacetic anhydride (21.0 g, 0.100 mmol) rapidly at 0° C. The reaction was completed after a few minutes. Water was added and the aqueous layer was extracted with methylene chloride. The combined organic layers were washed with water, brine and dried over magnesium sulfate. After filtration, the filtrate was concentrated to give 9.18 g of 3-cyano-5-methylpyridine crude, which was used in the next step without purification.

1. waitThe reaction was completed after a few minutes
2. extractionthe aqueous layer was extracted with methylene chloride
3. washThe combined organic layers were washed with water, brine
4. dry with materialdried over magnesium sulfate
5. filtrationAfter filtration
6. concentrationthe filtrate was concentrated