反应详情

温度

80 °C

Potassium carbonate (78 mg) and 2-oxa-6-azaspiro[3.3]heptane (30 mg) were added to a methanol/DMF (1 ml/2 ml) solution containing 2-chloro-5-nitropyridine (30 mg), followed by stirring at 80° C. for 3 hours. The reaction solution was adjusted to room temperature, and water was added, followed by extraction with ethyl acetate. The resultant was washed with saturated saline and dried over anhydrous sodium sulfate, the solvent was distilled away under reduced pressure, the obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=1:1 to 1:4), and a white solid of 6-(5-nitropyridin-2-yl)-2-oxa-6-azaspiro[3.3]heptane (23 mg) was thus obtained.

1. customwas adjusted to room temperature
2. extractionfollowed by extraction with ethyl acetate
3. washThe resultant was washed with saturated saline
4. dry with materialdried over anhydrous sodium sulfate
5. distillationthe solvent was distilled away under reduced pressure
6. customthe obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=1:1 to 1:4)