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温度

0 °C

A solution of methyltriphenylphosphonium bromide (4.98 g, 13.9 mmol) in anhydrous tetrahydrofuran (130 ml) at 0° C. and under inert atmosphere was added with a 1.6M butyl lithium solution in hexane (8.69 ml) and the mixture was left under stirring at 0° C. for 2 h. After that, a solution of 4-(4-phenylbutoxy)benzaldehyde (2.5 g, 9.84 mmol) in tetrahydrofuran (10 ml) was added and the mixture was left under stirring at room temperature for 36 h, then carefully added with water (20 ml) and extracted with ethyl ether (4×50 ml). The organic extracts were dried and the solvents were evaporated off under reduced pressure. The resulting crude was purified by chromatography through a silica gel column, eluting with petroleum ether:ethyl ether, 95:5, thereby recovering 4.20 g of the title compound (62% yield).

1. waitthe mixture was left
2. waitthe mixture was left
3. stirringunder stirring at room temperature for 36 h
4. extractionextracted with ethyl ether (4×50 ml)
5. customThe organic extracts were dried
6. customthe solvents were evaporated off under reduced pressure
7. customThe resulting crude was purified by chromatography through a silica gel column
8. washeluting with petroleum ether