The product was then purified by flash chromatography and analyzed by IR‚ 1H NMR and 13C NMR. The synthesis of piperonylontitrile was successful. There was a yield of a pale yellow crystal of 36%. The average recovery is 51% with there being a range from 0-94 %1. A reason for a smaller yield than notable reported could have been due
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Although the yield of our reaction was mediocre‚ the purity of the sample (as analyzed by 1H and 13C NMR) was poor. There are many factors that may have caused poor purity‚ of which include reaction incompletion during exposure to microwave radiation‚ poor mixing‚ and poor product isolation during column chromatography. As seen in the 1H NMR spectrum‚ impurity peaks (>10%) corresponding to methyl (triphenylphosphoranylidene) acetate‚ acetone‚ ethyl acetate‚ and hexane
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Abstract: The purpose of this lab is to prepare phenylmagnesium bromide‚ a Grignard reagent‚ and react it with benzophenone to give triphenylmethanol. Once made‚ the Grignard reagent will do a nucleophilic attack on the carbonyl carbon of the ketone‚ benzophenone. The result is an alkoxide that is then protonated to give the alcohol‚ triphenylmethanol. The purity of the final product will then be considered by melting point and IR spectroscopy. Final purified triphenylmethanol weighed 8.02 grams
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use the manufactured Grignard reagent to synthesize the alcohol‚ triphenylmethanol‚ by reacting with benzophenone and protonation by H3O+. The triphenylmethanol was purified by recrystallization. The melting point‚ Infrared Spectroscopy‚ 13C NMR‚ and 1H NMR were used to characterize and confirm the recrystallized substance was triphenylmethanol. Introduction A Grignard reagent is a type of organometallic‚ which consists of a bond between a metal and a carbon. There are three types of carbon-metal
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H2SO4 as another solvent‚ synthesize salicylic acid. The final step involves purify the product to produce as pure a sample of salicylic acid as possible. This process allowed for the successful production of 1.406g salicylic acid‚ an 82.70% yield. The NMR and IR both produced images that correlate with the known spectrums indicating a pure product. The melting point range was slightly wider‚ though did encompass the accepted melting point values. Discussion: Reaction OH O OCH3 2) H2SO4 1) 2NaOH OH
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Alkylation Reaction Friedel-Crafts Alkylation Reaction Preparation of 1‚ 4-Di-t-butyl-2‚ 5-dimethoxybenzene Microscale Experiment Leah Monroe April 8‚ 2003 Organic Chemistry Lab II Experiment performed on March 20 and 25‚ 2003 Lab Partners (NMR only): Shannon Land and Jamie Yeadon Abstract: In this experiment‚ 1‚4-dimethoxybenzene reacted with t-butyl alcohol to form 1‚ 4-Di-t-butyl-2‚ 5 dimethoxybenzene via a Friedel-Crafts Alkylation mechanism. A small amount of 1‚4-dimethoxybenzene
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an Unknown Organic Compound The objective of this lab was straightforward. We were given an unknown compound and we were to perform an IR spectroscopy and as well as NMR spectroscopy. With the IR spectroscopy‚ I was able to name the functional groups I have on my compound and further confirmed my assumptions by looking at the NMR spectroscopy after. The unknown number I was given was number 203. The molecular weight of the compound was 121. From the molecular weight‚ I calculated the molecular formula
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magnesium and ether. Phenylmagnesium bromide was then transformed into a tertiary alcohol called triphenylmethanol‚ through addition of another compound called benzophenone‚ as well as additional ether. The end product of triphenylmethanol was analyzed via NMR and IR. Figure 1: Preparation of the Grignard agent by combining bromobenzene with magnesium and ether to produce phenylmagnesium bromide. Figure 2: Production of triphenylmethanol by combining benzophenone and the Grignard reagent. Introduction
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molar mass (g/mol) To further enforce the conclusions drawn regarding the acids identity from the titration (crotonic acid for my sample)‚ NMR spectra were given for the unknown acid. A little bit of research reveals that the NMR spectra for crotonic acid is exactly what was given on the Human Metabolome Database (http://www.hmdb.ca/). Copies of their NMR spectra are printed and though this data is pretty convincing‚ it can only be reinforced. Three more tests were conducted. The
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RAPPTH-Co (II): H1 NMR: δ2.61 (s‚CH3‚3H)‚2.49(s‚CH3‚3H)‚6.40- 7.97 (m‚pyH‚7H )‚ 9.98(s‚ OH.IH)‚ 11.29ppm (s‚ NH‚ 1H). IR (KBr): 3480(OH‚ water)‚ 3227(ph O-H)‚ 1585(C=N)‚ 3349(N-H)‚ 1666 (C=O)‚ 554(M-O)‚ 436 cm-1 (M-N).RAPPTH-Cu (II): H1 NMR: δ2.73 (s‚CH3 ‚3H)‚2.50 (s‚CH3‚ 3H)‚ 6.42- 7.95(m‚pyH‚7H)‚ 10.14 (s‚OH.IH)‚ 11.30ppm (s‚NH‚1H). IR (KBr): 3420(OH‚ water)‚ 3230(ph O-H)‚
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