Organic 2 Review Problem 313

Organic 2 Review Problem 313 - P REPARATIONS 297 (Fig. 4...

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PREPARATIONS 297 (Fig. 4i(A) and (B), p. 65) into which the ethereal extract is al- lowed to run from a dropping-funnel at approximately the rate at which the solvent is distilling. When the ether has been removed, fit a capillary tube and thermometer, and continue the distillation at water-pump pressure. The diethyl ester of colli- dine-3,5-dicarboxylic acid (II) distils as a pale golden oil, b.p. i76-i78°/i4 mm. Yield, 5 g. from 6 g. of the ester (I). Collidine-3,$-dicarboxylic acid. Boil a mixture of 5 g. of the ester (II) and 50 ml. of 15% ethanolic potash under reflux for 30 minutes. The dipotassium salt crystallises during the boiling and during the subsequent cooling. Filter off the potassium salt at the pump and wash it with a small quantity of ethanol. Dilute the filtrate with about an equal volume of ether to precipitate a further small crop of the salt. Yield of combined crops: 4-5 g. from 5 g. of the ester (I). To obtain the free acid, add a solution of 2 g. of the potassium salt in 15 ml.
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This note was uploaded on 09/19/2011 for the course CHM 2211 taught by Professor Castalleano during the Fall '06 term at University of Florida.

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