反应详情

In 20 ml of dry benzene was dissolved 2.28 g of cis-2,2-dimethyl-3-(2,2-dichlorovinyl)cyclopropanecarbonyl chloride, followed by addition of 2.34 g of 3-(4-chlorophenoxy)benzyl alcohol and 1.58 g of pyridine. The mixture was stirred at room temperature overnight. Thereafter, the reaction mixture was washed with dilute hydrochloric acid and water, dried over anhydrous magnesium sulfate and distilled under reduced pressure to remove a low-boiling fraction, whereby an oily product was obtained as a residue. This oil was purified by preparative liquid chromatography [column: Waters Associates' Prep LC/System 500, Prep PAK® 500/SILICA; solvent system: diisopropyl ether:n-hexane=6:94, v/v]. The above procedure yielded 3.91 g of 3-(4-chlorophenoxy)benzyl cis-2,2-dimethyl-3-(2,2-dichlorovinyl)cyclopropanecarboxylate (yield 92%).

1. washThereafter, the reaction mixture was washed with dilute hydrochloric acid and water
2. dry with materialdried over anhydrous magnesium sulfate
3. distillationdistilled under reduced pressure
4. customto remove a low-boiling fraction, whereby an oily product
5. customwas obtained as a residue
6. customThis oil was purified by preparative liquid chromatography [column: Waters Associates' Prep LC/System 500, Prep PAK® 500/SILICA; solvent system: diisopropyl ether:n-hexane=6:94, v/v]