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Molecules 2016, 21, 24 7 of 11 3. MaterialsandMethods 3.1. General Amine Protection The required quantity of amine was added to a round-bottom flask before the addition of any other component. A CO2 atmosphere was then introduced into the closed vessel via a CO2 gas cylinder equipped with a low pressure regulator for approximately 5 min resulting in the exothermic formation of solid white powders. The reaction solvent was then added with additional CO2 being bubbled through the solution for a further 3 min. The original volume of the solution was made up with pure solvent after the CO2 bubbling in order to preserve concentrations. The reactions with protected amines were carried out under a CO2 atmosphere. 3.2. General Amine De-Protection Carbamate solutions of the alkylamines were de-protected using indirect heat and thermostat control with stirring. An ice-bath cooled condenser was attached to the top of the reaction vessel while a steady stream of nitrogen was introduced to aid the reversal. This was carried out for 10 min, after which fresh solvent was added to maintain the reaction concentration after nitrogen saturation. This procedure was used in attempt to convert carbamates back to the original amines. The de-protected amines were then employed in the urea/imine synthesis to ensure complete de-protection and no loss of reactivity. 3.3. General Characterization An aliquot of the reaction mixture (1.5 mL) was taken from each reaction vessel and injected into an Agilent 7695A GC using the Agilent 7683B automatic liquid sampler (Agilent Technologies, Santa Clara, CA, USA). The inlet temperature was set at 300 ̋C with a pressure of 16 psi, the oven at 80 ̋C with a heating rate of 20 ̋C/min to 250 ̋C. The FID was set at 300 ̋C. A calibration curve for benzophenone (BP) was created by plotting the integral of the BP peak vs. known concentrations of BP (Rt = 14.5 min). Melting points were determined from DSC spectra obtained using a Thermal Analysis SDT Q600 (TA Instruments, New Castle, DE, USA) equipped with alumina pans. A steady heating rate of 5 ̋C/min was maintained to 350 ̋C with a nitrogen purge of 100 mL/min. IR spectra were collected on a Nexus 870 spectrometer (Nicolet Instrument Corporation, Madison, WI, USA) with a 4 cm ́1 resolution using 64 scans. A fixed angle single reflection 60 ̋ hemispherical Ge crystal plate, equipped with an ATR pressure clamp, was placed in a sample compartment. The output signal was collected using a deuterated triglycine sulfate (DTGS) room temperature detector. 1H-NMR spectra were obtained on a Bruker 300 MHz in CDCl3 (Bruker Biospin Corporation, Billerica, MA, USA). 3.4. Synthesis of n-Alkyl, n-Phenyl Urea Exactly 50 μL (0.0545 g, 0.46 mmol) of phenyl isocyanate was added dropwise to a solution of alkylamine (0.92 mmol) in 2 mL of dry CHCl3 at 0 ̋C. The resulting solution was stirred for 60 min at room temperature and then precipitated into 25 mL of pentane. The product was isolated as a white powder via filtration and washed with several portions of pentane before being dried under vacuum at 50 ̋C. The products isolated from the alkylcarbamates were alternatively re-dispersed in dry CHCl3 and underwent thermal treatment to remove any residual carbamates. The ureas were then re-crystallized in pentane again and isolated via filtration to determine yield (Scheme 2a). 3.5. Synthesis of n-Propyl, Benzophenone(BP) Imine Propylamine (5 mmol) was added to 5 mL of dry methanol, followed by 2.5 mmol benzophenone (BP) and 3.3 mmol titanium(IV)-isopropoxide. The solution was stirred under nitrogen at room temperature while aliquots were taken at 3, 6 and 24 h for GC analysis and ATR-FTIR monitoring.PDF Image | Amines vs Nucleophilic Substitution Reversible Reaction CO2
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