反应详情

To a solution of 2-chloro-5-nitroisonicotinic acid (Intermediate 25A) (0.64 g, 3.17 mmol) in DMF (15 mL) under nitrogen was added sodium carbonate (1.0 g, 9.51 mmol). Reaction cooled in an ice bath and methyliodide (1.35 g, 9.51 mmol) was added dropwise. After complete addition, reaction allowed to warm to room temperature and stirred overnight under nitrogen. The reaction mixture was filtered and concentrated. The resultant crude material was purified by a 20 g silica column eluting with 40% ethylacetate in hexane to afford methyl 2-chloro-5-nitroisonicotinate (0.62 g, 2.86 mmol).

1. customReaction
2. temperaturecooled in an ice bath
3. additionAfter complete addition, reaction
4. filtrationThe reaction mixture was filtered
5. concentrationconcentrated
6. customThe resultant crude material was purified by a 20 g silica column
7. washeluting with 40% ethylacetate in hexane