Experimental Organic Chemistry

Cover Experimental Organic Chemistry
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(See Fig. 14, page 25. ) At the end of this time, arrange the apparatus for distillation, using a water condenser and having a thermometer to record the temperature of the vapor. Distil into a flask; when the temperature registers 100, collect separately about 1 cc. Of the distillate and add it to about 5 cc. Of water. If the mixture does not separate into two layers, stop the dis- tillation. Shake the distillate in the flask with 30 cc. Of water, and add solid sodium carbonate until a drop of ...the ester is neutral to moist litmus paper. Transfer to a separatory funnel, draw off the water, and shake the ester twice with a saturated solution of calcium chloride, using 50 cc. Each time. Draw off the ester into a distilling flask, add about one-fourth its volume of an- hydrous calcium chloride, close the flask and cover the side-arm with corks, and let stand for at least 1 hour. Distil from a water-bath. Note the boiling-point and the weight of ester ob- tained, and calculate the percentage yield from the acetic acid used.

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