Abstract/Intro:Purpose of experimentation was to create, optimize, and standardize a microwave assisted one pot reaction to transform aldehydes into nitriles using hydroxylamine hydrochloride, phthalic anhydride, and N-methylmorpholine.
Procedure:Place hydroxylamine hydrochloride (1.1 mmol), N-methylmorpholine (1.2 mmol), phenylacetaldehyde (1.0 mmol), and 1,2-dichloroethane (1-2 ml) in a concical flask, test tube, or beaker. Place the reaction vessel in an unmodified domestic microwave and irradiate at high power for 1 to 2 minutes or until all starting material is reacted into aldoximes. (This can be observed via TLC in a 3:7 solution of ethyl acetate:hexane). Then add the phthalic anhydride (1.2 mmol) and microwave for 3 to 4 minutes at high power, or until all the aldoxime is completely reacted (TLC in a 3:7 solution of EtOAc:Hexane). The product would then undergo a work up procedure consisting of dilute sodium hydroxide solution to remove phthalic acid completely and then potable water. After working up, sodium sulfate is added to the solution to remove water molecules; the solution was then filtered. The filtered solution was then evaporated under reduced pressure and then dried in a vacuum pump. Melting point tests and Infrared Spectrophotometric Analyses were performed to confirm the
product.
Conclusion:Phenylacetaldehyde was converted to benzyl cyanide in 8 Minutes at the highest effect in a domestic microwave oven with 97% yield of the product.
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Overall yield (to the amphetamine): 88.5 %
Reference:Microwave Assisted Rapid Transformation of Aldehydes Into Nitriles by Frank P. De Paoli
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