Magnesium turnings (7.2 g, i.e. 0.3 g-atom), which had been washed with absolute alcohol and dry ether, dry ether (150 ml), and an iodine crystal were introduced into a one-liter three-necked round-bottomed flask fitted with mercury-sealed stirrer, dropping funnel, and reflux condenser protected by a calcium chloride tube. Over a period of 90 minutes a solution of 60 g (0.38 mole) of freshly distilled bromobenzene in 100 ml of dry ether was added from the dropping funnel (Note 1). When the whole of the bromobenzene had been added, the mixture was boiled gently in a water bath for four hours until dissolution of the magnesium was substantially complete. The contents of the flask were then cooled with ice and salt and were stirred continuously for 40–50 minutes while a solution of 27.3 g (0.27 mole) of freshly distilled 2-furaldehyde in 150 ml of dry ether was added.
KeywordsReflux Condenser Vertical Tube Grignard Reagent Substance Resinifies Furoic Acid
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