反应详情

温度

0 °C

A mixture of pyrrolidine (0.910 g, 10.7 mmol) in dry DMSO and NaH (0.385 g, 16.0 mmol) was stirred for 30 minutes at 0° C., after which a sample of 2,4,6-trichloropyridine (1.75 g, 9.63 mmol) was added. This reaction mixture was stirred at room temperature for 4 hours, after which time ice cold water was added to quench the reaction. The reaction mixture was then extracted with ethyl acetate, and the extract was washed 3-4 times with water. The organic layer was dried over sodium sulphate and concentrated. The residue was purified by column chromatography over 100-200 mesh silica gel. Elution of the column with 20% acetone in hexanes gave the pure product as a colorless solid (yield: 75%).

1. stirringThis reaction mixture was stirred at room temperature for 4 hours
2. additionafter which time ice cold water was added
3. customto quench
4. customthe reaction
5. extractionThe reaction mixture was then extracted with ethyl acetate
6. washthe extract was washed 3-4 times with water
7. dry with materialThe organic layer was dried over sodium sulphate
8. concentrationconcentrated
9. customThe residue was purified by column chromatography over 100-200 mesh silica gel
10. washElution of the column with 20% acetone in hexanes