反应详情

温度

0 °C

To a solution of 2-dimethylaminoethanol (5.60 g, 62.8 mmol) in hexane (80 ml) was added dropwise 1.6N hexane solution of n-butyl lithium (78.5 ml, 125 mmol) under ice-cooling, and stirred at 0° C. for 30 minutes. Then, 4-phenylpyridine (3.24 g, 20.8 mmol) was added thereto, and stirred at 0° C. for 1 hour. After cooling the reaction solution to −78° C., a solution of carbon tetrabromide (25.0 g, 75.4 mmol) in hexane (40 ml) was added thereto, and stirred at −78° C. for 1 hour, then at room temperature for 1 hour. To the reaction solution was added water under ice-cooling, and extracted with ether. The extract was dried over anhydrous magnesium sulfate, and the solvent was distilled away under reduce pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1) to give the titled compound 2.21 g (45.4%) as solid product.

1. temperaturecooling
2. stirringstirred at 0° C. for 1 hour
3. temperatureAfter cooling the reaction solution to −78° C.
4. stirringstirred at −78° C. for 1 hour
5. waitat room temperature for 1 hour
6. temperaturecooling
7. extractionextracted with ether
8. dry with materialThe extract was dried over anhydrous magnesium sulfate
9. distillationthe solvent was distilled away
10. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1)