Hydrochloric Acid → HCID 67584087, compound

Participants

Reaction Conditions

Reaction Steps

A Grignard reagent prepared from 3-fluoro-4-trifluoromethoxyphenylbromide (200.0 g, 772 mmol) and dried Mg (18.8 g, 774 mmol) in ether was cooled down to -50° C. in a nitrogen atmosphere, followed by dropwise adding thereto a 100 ml ether solution of ethylene oxide (100 g, 2.27 mol), stirring the reaction solution at 0° C. for 2 hours, adding the resulting reaction product to 6N HCl, extracting the product with toluene, washing the extraction solution successively a saturated aqueous solution of sodium bicarbonate and water, drying over the organic layer over magnesium sulfate, distilling off the solvent, adding to the residue, 47% hydrogen bromic acid (300 ml) and xylene (300 ml), refluxing the mixture for 9 hours, while removing water formed by the reaction by means of Dean-Stark, adding water (500 ml) to the resulting reaction product, extracting the resulting product with toluene, washing the extraction solution successively with a saturated aqueous solution of sodium bicarbonate and water, distilling off the solvent, and distilling the residue under reduced pressure, to obtain 3-fluoro-4-trifluoromethoxyphenetylbromide (68.3 g, 238 mmol). Yield: 30.7%.

Provenance & Evidence