Organic Lab Reactions 257

Organic Lab Reactions 257 - 252 THE PREPARATION OF...

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252 THE PREPARATION OF UNSYMMETRICAL BIARYLS liquid. After no more nitrouB fumes are evolved, the flask is cooled to 40° and 150 g. of dry sodium chloride is added. The side arm of the flask is connected to a tube running down to the bottom of a 10-inch test tube immersed in an acetone-dry ice mixture. The top of the distilling flask is closed with a rubber stopper, and the water bath is warmed slowly to about 80° and kept there until no more yellow-ora.nge fumes of nitrosyl chloride come off from the mixture. The red liquid NOC1 which is col- lected weighs 60 g. Pure nitrosyl chloride boils at —5.5°. Nitrosyl Chloride Procedure (B-2) ^-Terphenyl. 8 '" To a stirred solution of 10 g. of diacetyl-1,4- phenylenediamine in a mixture of 150 cc. of glacial acetic acid and 75 cc. of acetic anhydride containing 12 g. of anhydrous potassium acetate and • 1 g. of phosphorus pentoxide at 8° is added dropwise a solution of 8 g. of nitrosyl chloride in acetic anhydride. The mixture is poured onto ice
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