反应详情

To a mixture of 5-bromo-2-methoxymethoxybenzyl cyanide (2.10 g), 2-bromo-3-methoxymethoxypyridine (1.79 g), sodium p-toluenesulfinate (0.44 g) and THF (30 ml) was added, at room temperature, 60% sodium hydride (0.69 g), followed by heating for 2 hours under reflux under argon atmosphere. The reaction mixture was poured into a saturated aqueous saline solution, which was subjected to extraction with ethyl acetate. The extract solution was washed with a saturated aqueous saline solution, dried (anhydrous sodium sulfate), and concentrated. The concentrate was purified by means of a silica gel column chromatography (eluted with ethyl acetate/hexane) to give 2-(5-bromo-α-cyano-2-methoxymethoxybenzyl)-3-methoxymethoxypyridine (2.58 g), whose physical properties and spectrum data are shown in Table 9 and Table 12.

1. additionwas added, at room temperature
2. temperatureby heating for 2 hours
3. temperatureunder reflux under argon atmosphere
4. additionThe reaction mixture was poured into a saturated aqueous saline solution, which
5. extractionwas subjected to extraction with ethyl acetate
6. washThe extract solution was washed with a saturated aqueous saline solution
7. dry with materialdried (anhydrous sodium sulfate)
8. concentrationconcentrated
9. customThe concentrate was purified by means of a silica gel column chromatography (eluted with ethyl acetate/hexane)