Tert-Butydrochlorimetric Analysis

Abstract: The purpose of this experiment is to use the apparatus shown in figure 7-1 of experiment 6 found in the lab manual, to synthesize [1,3,5-C6H3(CH3)3]Mo(CO)3.(2016 Oleg) With this, characterization of the molecule can be accomplished using the infrared spectrum and NMR spectrum of the synthesized compound. It was found in the IR spectra of the product, that suitable stretches were found associated with the C-O bonds of mestylene and molybdenum. With One strong spectra was found at 1855.3973 cm-1 , one medium strength spectra was found at 1942.6002 cm-1 , and one weak spectra of C-O stretch was found at 1298.8638cm-1 . The 1H NMR spectrum of the product showed peaks at δ 2.28 and 5.25, while the H NMR spectrum of mesitylene gave peaks at δ

After synthesizing tert-butyl chloride, the melting point on the compound was found to be 47˚C. According to literature, tert¬-butyl chloride has a melting point of 51˚C, apart from a little bit of deviation, this shows that the correct compound was created. The percent yield obtained for the synthesis of tert-butyl chloride was 47.42%. This could have been due to errors that occurred in the lab. When moving the solution from one test tube or graduated cylinder to another some of the solution may still be left in the tube which lowers the percent yield. Also when working with a simple distillation setup, the vial is not distilled to dryness therefore some of the solution is not collected. Some of the solution can also be trapped on the side

9-anthraldehyde and (carbethoxymethylene)triphenylphosphorane were reacted together using the Wittig reaction to produce E-3-(9-Anthryl)-2-propenoic acid ethyl ester. .100 g of 9-anthraldehyde and .180 g of (carbethoxymethylene)triphenylphosphorane were used. 9-anthraldehyde was a green powder while (carbethoxymethylene)triphenylphosphorane was a white powder. Both were added together into a 3.00 mL conical vial with a magnetic spin valve. The vial was inserted into a 120 C sand bath to melt the reagents. Once the reagents melted, they were stirred for 15 minutes (2:30 pm-2:45 pm). After stirring, the vial was removed to cool to room temperature. 3.00 mL of hexanes were added to the vial and the suspension was stirred. The solvent was removed

After 10 minutes the reaction liquid was separated from the solid using a vacuum filtration system and toluene. The product was stored and dried until week 2 of the experiment. The product was weighed to be 0.31 g. Percent yield was calculated to be 38.75%. IR spectra data was conducted for the two starting materials and of the product. Melting point determination was performed on the product and proton NMR spectrum was given. The IR spectrum revealed peaks at 1720 cm-1, which indicated the presence of a lactone group, and 1730 cm-1, representing a functional group of a carboxylic acid (C=O), and 3300cm-1, indicating the presence of an alcohol group (O-H). All three peaks correspond with the desired product. A second TLC using the same mobile and stationary phase as the first was performed and revealed Rf Values of 0.17 and 0.43for the product. The first value was unique to the product indicating that the Diels-Alder reaction was successful. The other Rf value of 0.43 matched that of maleic anhydride indicating some

Using SN1 reaction mechanism with hydrochloric acid, t-Pentyl alcohol was converted to t-Pentyl chloride in an acid catalyzed reaction. The reaction took place in a separatory funnel designed to separate immiscible liquids. The crude product was extracted by transferring a solute from one solvent to another. The process of washing the solutions by phase transfer was used in order to remove impurities from the main solvent layer. Finally, the crude product was dried with anhydrous Calcium chloride and purified once more by simple distillation technique.

A pre-weighed (0.315g) mixture of Carboxylic acid, a phenol, and neutral substance was placed into a reaction tube (tube 1). tert-Butyl methyl ether (2ml) was added to the tube and the solid mixture was dissolved. Next, 1 ml of saturated NaHCO3 solution was added to the tube and the contents were mixed separating the contents into three layers. Once this was completed

The reaction is carried out in saturated aqueous ammonium chloride solution. Thus no special drying of solvents, reagents, or glassware is required. The reaction mechanism for this experiment can be seen below (Fig. 2)

The reaction took place in a conical vial and .2mL of each of the reactant samples were added to it along with some 95% ethanol. Two drops of NaOH were added shortly after and stirred at room temperature for fifteen minutes. The vial was cooled in and ice bath and crystallized. Vacuum filtration was performed to filter the crude product. The crude product was recrystallized using methanol and filtered again. We made one change to the procedure and instead of using .7mL of ethanol we

Olmsted, John III; Williams, Greg; Burk, Robert C. Chemistry, 1st Canadian ed.; John Wiley and Sons Ltd: Mississauga, Canada, 2010, pp 399 - 406

Complexation of porphyrin with the metal will cause the shifts of Q bands in the UV-Vis spectra in the range of 500-700 nm as shown in Figure 2.7. This can be observed by the disappearance of two Q bands out of four as the porphyrin undergoes the change from D4h symmetry to D2h symmetry (Rita Giovannetti, 2012). The Q-bands were denoted as α and β. The coordination of porphyrin to Ni(II), Sn(IV) or Pd(II) which can form stable square planar complexes generally consists of a higher α peak (Figure 2.7 (A)), while the coordination of porphyrin to Cd(II) which forms a complex that can easily be displaced by protons will show a higher β peak (Figure 2.7(B)).

Pyridazinone are potent medicinal scaffolds and exhibit a full spectrum of biological activities. This review throws light on the detailed synthetic approaches which have been applied for the synthesis of pyridazinone. This has been followed by an in depth analysis of the pyridazinone with respect to their medicinal significance. This follow-up may help the medicinal chemists to generate new leads possessing pyridazinone nucleus with higher

A Magritek NMR spectrometer along with MNOVA software was used to obtain the 1H NMR spectrum by inserting an epi tube containing CDCl3 solvent with 60mg of dissolved 4-bromo-N- 4-(chlorophenyl)methylene]-benzenamine from the purest sample obtained from the reaction using molecular sieves into the spectrometer. Once the tube was inserted, proton protocol was selected with parameters of CDCl3 as the solvent and it underwent a quickscan to acquire the spectrum. When the scan was completed the spectrum was transferred to the MNOVA software for process, label, integrate, and summarized the collected peaks. The IR spectrum was obtained using a different machine since the Magritek NMR spectrometer used only produced 1H and 13C NMR spectrums from samples placed in an epi tube.

3r0To6cb8el)xTc029.80. 1c20(l7) 0.8 e0c(o4,sen1t 07(.0w)1T01e(js). T0 3T76(l) c( ie9.0T /0F z1/0F. 010T.f0 Ts0f.37T6Tc(Tz/F0.OT0700co0j)90,j.()30.)c8.s0Tc(02 67T T(Iw105 8T25T0c(ecT j3")0T 2c.3(1)4.Tw-0a. 72T0.c( exsa)7 T(fj) .Trespn)1si2hTB6230 T8r0 0 cT.0(l) T9.5090j3.i910.000cT 280 Td0. 0 Tw9 .0Tf0.61(Tc,)r 0 0 c(,ra]ilTBT3 Tr0. 0 Ts0.608062..68d;0r3Bhaj)0002e(\ d 8T 31 . 1. 5(n Tcxp iKl i'. T T0. ( e T4 80 0t153 0 2 .iEnlej iEe) Tj4. 20Tc(jioint)537oint)5(e)T6iTr9g3o3 in r 17 cw37 c(nieh.0 4b96 rg1Tj3.3300.Tese.)01(63.0T0.Te0607T 2 .2( ) j4d 2 w r 0 c Tcw0 3 (f Tsi fi ) j4 2 Tw0.583 T5.461 60Tw0.150.T)Ti0 d0 0 Tw9c( deTz/F0 Tc(T72T6.TfT50 s037 c( 86 w129.120 6(e) Tj3a)90,Tc() . a) Tj0. 0 05 .0Tj0.000TlTc() 0. 0 1038 0.480 Tc4(s))6Te4T83(T1.T)9T10)Tc(, 1 67 ) j el j469 w 6 c6 a ) 10 31 Tj hi\ nls) Tj5.708Tjkn b213)Tw0j.5103o(4)TcjT1fo40e. Td0. 0 Tw9r.0 0 870. g1Tl190 Tc0190.480 Tw0p( deTz/F0 10. 0 Tf0 Ts0.376 Tc(2867 Tw140. 0 Tec( ) Tj3.0 Tc(,) .0 9 a) Tj0. 0 xa42 i)j1iasohie) Tj4. 20 Tw0 .265 Tc87 0. 01o09(n) Tjst:iloi>0.

IR (KBr): νmax (cm-1): 2962 (Ar-H), 1664 (C=O), 1604 (C=C), 819 (C-Cl). 1H-NMR (400 MHz, DMSO-d6): δ ppm, 1.20 (d, 3H, CH3), 2.48-2.96 (m, 1H, CH), 7.74 (d, 1H, CH, J=17 Hz), 7.84 (d, 1H, CH, J=17 Hz), 7.12-8.17 (m, 8H, Ar-H). LCMS (m/z): 285.2 (M++1). C H N analysis: Calculated for C18H17ClO: C, 75.92; H, 6.02; Found: C, 75.90; H, 6.05%.

Abstract: The reactions of 2-amino-3-cyano-4.6-diarylpyridines with formic acid, glacial acetic acid, benzoyl chloride, formamide and acetamide afforded 5-(5-substitutedfuran-2-yl)-7-(4-substitutedphenyl)-3H-pyrido[2,3-d] Pyrimidin-4-one , 2-methyl-5-(5-substitutedfuran-2-yl)-7-(4- substituted phenyl)-3H-pyrido[2,3-d] pyrimidin-4-one, 5-(5-substitutedfuran-2-yl)-7-(4-substitutedphenyl)-2-phenyl-3H-pyrido[2,3-d] pyrimidin-4-one, 5-(5-substitutedfuran-2-yl)-7-(4-substituted phenyl)-pyrido[2,3-d] pyrimidin-4-ylamine, 5-(5-substitutedfuran-2-yl)-7-(4-substitutedphenyl)-2-methyl-pyrido[2,3-d] pyrimidin-4-ylamine, respectively. The newly synthesized heterocycles were characterized by elemental analysis, IR, 1H-NMR, 13C-NMR and mass spectral data. Compounds have been screened for their antibacterial, antifungal and anticancer activities.