反应详情

First, 0.39 g of 4-(2,6-diethyl-4-(3,3-dichloro-2-propenyloxy)phenoxy)butyloxyacetaldehyde was dissolved in 10 ml of anhydrous methanol, to which 5 mg of ammonium chloride was added, and the mixture was heated under reflux for 3 hours After left alone for cooling, the reaction mixture was mixed with 10 ml of saturated aqueous sodium hydrogencarbonate solution. The methanol was distilled out, and the residue was extracted twice with diethyl ether. The diethyl ether layers were combined, washed with water, dried over anhydrous magnesium sulfate and then concentrated to give a crude product. The crude product was subjected to silica gel chromatography, which afforded 0.31 g of 3,5-diethyl-1-(3,3-dichloro-2-propenyloxy)-4-(4-(2,2-dimethoxyethoxy)butyloxy)benzene (yield, 71%), nD24.0 1.5068.

1. additionwas added
2. temperaturethe mixture was heated
3. temperatureunder reflux for 3 hours
4. waitAfter left alone
5. temperaturefor cooling
6. distillationThe methanol was distilled out
7. extractionthe residue was extracted twice with diethyl ether
8. washwashed with water
9. dry with materialdried over anhydrous magnesium sulfate
10. concentrationconcentrated
11. customto give a crude product