Organic Lab Reactions 151

Organic Lab Reactions 151 - 146 THE FORMATION OF CYCLIC...

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146 THE FORMATION OF CYCLIC KETONES a suspension of 91 g. (0.38 mole) of a,7-diphenylbutyric acid in 200 cc. of dry benzene. 1166 After the vigorous reaction subsides and the reactants are nearly completely dissolved, the mixture is heated for a few minutes on a steam bath. A condenser and receiver are then set for reduced-pres- sure distillation, and all the volatile material is removed at the water pump at 100° or less to avoid discoloration of the acid chloride. The residual oily acid chloride is transferred with 380 cc. of dry thiophene- free benzene into a 1-1. three-necked flask equipped with a condenser (calcium chloride tube), a mercury-sealed wire stirrer, 112 and a rubber- tubed addition flask (p. 145) containing 53 g. (0.4 mole) of aluminum chloride. (The reaction temperature is more readily controlled with lumpy aluminum chloride than with finely powdered grades.) The aluminum chloride is added to the stirred solution at room temperature over a period of one-half hour (external cooling is sometimes necessary). The mixture is then heated for one-half hour each at 40° and 60°. After
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This note was uploaded on 11/20/2011 for the course CHM 2210 taught by Professor Reynolds during the Fall '01 term at University of Florida.

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