反应详情

To a suspension of 5-bromo-4-chloro-2-methoxymethoxybenzyl cyanide (10.4 g), 2-bromo-3-methoxymethoxy pyridine (7.81 g) and sodium p-toluenesulfinate (12.7 g) in THF (150 ml) was added, at room temperature, sodium hydride (3.63 g). The mixture was heated for 2 hours under reflux under argon atmosphere. The reaction mixture was cooled by aeration, which was poured into ice-water, followed by extraction with ethyl acetate. The organic layer was washed with a saturated aqueous saline solution, dried (anhydrous magnesium sulfate) and concentrated. The crystal obtained was washed with cyclohexane/isopropyl ether (5:1) to give 2-(5-bromo-4-chloro-α-cyano-2-methoxymethoxybenzyl)-3-methoxymethoxypyridine (10.9 g) (Compound C-15). The physical properties and spectrum data are shown in Table 9 and Table 12.

1. additionwas added, at room temperature
2. temperatureThe mixture was heated for 2 hours
3. temperatureunder reflux under argon atmosphere
4. temperatureThe reaction mixture was cooled by aeration, which
5. extractionfollowed by extraction with ethyl acetate
6. washThe organic layer was washed with a saturated aqueous saline solution
7. dry with materialdried (anhydrous magnesium sulfate)
8. concentrationconcentrated
9. customThe crystal obtained
10. washwas washed with cyclohexane/isopropyl ether (5:1)