Hydrochloric Acid → 2-[(Prop-2-en-1-yl)oxy]benzoyl chloride

関与物質

反応手順

To a 2000 ml four-necked reaction flask, equipped with a magnetic stirrer, thermometer, addition funnel, condenser and a nitrogen sweep, was added 281 grams of thionyl chloride (2.38 moles), 1 ml of dimethyl formamide, and 1000 ml of toluene. 356 grams of the allyloxybenzoic acid (2.0 moles) as prepared above was added over approximately 20 minutes. The reaction temperature was kept below 20° C. with an ice/water bath. The nitrogen sweep was connected to a trap, which contained 1000 ml of a 4 M aq. NaOH solution to react with SO2 and HCl that are formed during the reaction. After the addition was complete, the solution was stirred for 3 hours at room temperature and then heated to reflux. After 3.5 hours of reflux, it was cooled to room temperature. Solvent was distilled at atmospheric pressure because removal under reduced pressure caused severe bumping. After most of the solvent was removed, the residue was transferred to a 1000 ml flask equipped with a distillation head. The product was then vacuum distilled.

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