反应详情

The reaction mixture was cooled to room temperature and the residual pressure was released, and 100 ml of benzene was added into the autoclave to dissolve the oily portion. Then, the catalyst was removed by filtration, and the filtrate was sufficiently shaken and allowed to stand still to cause phase separation. Then, the obtained benzene layer was washed with 100 ml of water three times and benzene was removed by distillation under reduced pressure to give an oily product. From the results of the analysis of the oily product by gas chromatography according to the internal standard method, it was found that the oily product comprised 98.2% of 3-phenoxy-4-fluorobenzyl 2-(4-ethoxyphenyl)-2-methylpropyl ether and 0.7% of starting 3-phenoxy-4-fluorobenzyl 2-(3-chloro-4-ethoxyphenyl)-2-methylpropyl ether, and that the content of each of 3-phenoxy-4-fluorotoluene and 4-ethoxyneophyl alcohol formed by cleaving of the ether linkage was lower than 0.2%. Moreover, 0.8% of 3-phenoxybenzyl 2-(4-ethoxyphenyl)-2-methylpropyl ether presumed to have been formed by reduction of the fluorine atom was contained.

1. dissolutionto dissolve the oily portion
2. customThen, the catalyst was removed by filtration
3. customphase separation
4. washThen, the obtained benzene layer was washed with 100 ml of water three times and benzene
5. customwas removed by distillation under reduced pressure
6. customto give an oily product
7. customFrom the results of the analysis of the oily product by gas chromatography