Wednesday, February 27, 2013

Experiment 4

EXPERIMENT 4: PREPARATION OF PHENYLBENZOATE

In this experiment, you will pass water phenyl benzoate by the reaction of phenol with benzoyl chloride. Your aim in propaedeutic work of this sort must as pure a product as possible, in as high give in as possible.
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CAUTION:

BENZOYL CHLORIDE MUST BE KEPT IN THE FUME CUPBOARD AND NOT SPLIT ON THE hold OR CLOTHING. ITS VAPOUR IS HARMFUL AND PRODUCES AN EXTREMELY IRRITATING center ON EYES.

PHENOL IS VERY POISONOUS. AVOID CONTACT WITH THE SKIN.

PROCEDURE

deal a wide-mouthed scrap-stoppered bottle of about 250 cm3 capacity, and in it place 90 cm3 of 2M sodium hydroxide solution and 5g of phenol. Go to a grass cupboard and pour into the bottle with care 9 cm3 of benzoyl chloride. (Caution: This fluent must must be kept in the reek cupboard and not split on the hands or clothing. Its vapour is harmful and produces an extremely irritating effect on eyes.) Grease the stopper of the reaction bottle lightly with Vaseline and exchange it in the bottle, then, holding the stopper in place securely, crusade the bottle vigorously at intervals for a period of 15 minutes.

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At the end of this time collect the material obtained by suction filtration using a Buchner filtration apparatus, preferably still in fume cupboard, for trace of benzoyl chloride whitethorn still persist. Break up any lumps on the filter paper with a glass rod, but be careful not to puncture the paper. brush the solid well with water and discard the filtrate. Recrystallize the solid ester from ethanol, fetching care to see that just sufficient is use to rule out the ester separating as an oil at a temperature above its resolve point. The phenyl benzoate is obtained as white crystals. Which melt under 100oC. Use a hot water bath; do not passion the ethanol directly with a Bunsen flame because it may catch fire.

Dry your sample in the oven. Calculate the per centum yield of your sample and take the melting point. The temperature at which the crystals start-off melt...If you want to get a full essay, order it on our website: Orderessay



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