反应详情

The reaction mixture was cooled to room temperature and the gas was released. 100 ml of benzene was charged in the autoclave to dissolve an oil. An insoluble matter was filtered out. After washing with 20 ml of benzene, a resulting mother wash solution was shaken well and then left to stand to obtain a benzene layer. The benzene layer was washed with 100 ml of water three times. Benzene was distilled off under reduced pressure to obtain an oily product. According to gas chromatographic analysis by the internal standard method, the oily product contained 97.2% of 3-phenoxy-4-fluorobenzyl 2-(4-ethoxyphenyl)-2-methylpropyl ether and 1.0% of starting material 3-phenoxy-4-fluorobenzyl 2-(3-chloro-4-ethoxyphenyl)-2-methylpropyl ether. The amounts of 3-phenoxytoluene and 4-ethoxyneophyl alcohol formed by ether bond cleavage were each less than 0.1%. The amount of 3-phenoxybenzyl 2-(4-ethoxyphenyl)-2-methylpropyl ether formed probably due to the replacement of fluorine atom with hydrogen atom was only less than 0.5%.

1. dissolutionto dissolve an oil
2. filtrationAn insoluble matter was filtered out
3. washAfter washing with 20 ml of benzene
4. washa resulting mother wash solution
5. waitleft
6. customto obtain a benzene layer
7. washThe benzene layer was washed with 100 ml of water three times
8. distillationBenzene was distilled off under reduced pressure
9. customto obtain an oily product