反应详情

A solution of 2-chloro-6-methylnicotinic acid (1.00 g, 5.83 mmol) in tetrahydrofuran (10 mL) was successively added with N,O-dimethylhydroxyamine hydrochloride (910 mg, 9.33 mmol), N,N-diisopropylethylamine (3.00 g, 23.2 mmol) and DEPC (1.43 g, 8.77 mmol) on an ice bath, and the mixture was stirred at room temperature for 30 minutes. The reaction mixture was diluted with water, and extracted with ethyl acetate. The organic layer was washed with saturated brine, then dried over anhydrous sodium sulfate, and concentrated under reduced pressure, and the resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1) to obtain 2-chloro-N-methoxy-N,6-dimethylpyridine-3-carboxyamide as colorless solid.

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with saturated brine
3. dry with materialdried over anhydrous sodium sulfate
4. concentrationconcentrated under reduced pressure
5. customthe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1)