Answer Happy

Week 2 - Preparation and Isolation of the bisulfate salt of Lidocaine Remove the formed precipitate via vacuum filtration and rinse with 3 ml. of toluene. Transfer the filtrate to a separatory funnel and extract twice with 20 ml. portions of 3 M HCl. During the extraction, use vigorous shaking and frequent venting. Combine the two HCI fractions in an Erlenmeyer flask and add –25 ml. of 20% NaOH. Ensure the mixture is strongly basic (>10 pH) and cool in an ice bath. Transfer the cooled solution to a separatory funnel and extract with two 15 ml. portions of diethyl cther (using the first portion to rinse out your flask containing your original basic solutions.) Again, use vigorous shaking and frequent venting Wash the combined ether layers with 25 mL of DI water. Dry the organic layers with MgSO.. Gravity filter into a tared 100 ml round bottom flask. Remove the solvent on the rotovap and any residual solvent using the air drying system Salt formation: Dissolve the crude product in diethyl ether (10 mL of solvent per g of solute) and transfer to a beaker. Add 2 mL of 2.2 M sulfuric acid in ethanol per g of solute and an equal portion of reagent grade acetone to that of the diethyl cther you added previously. Cool the solution in an ice bath and stir/scratch the bottom of the beaker continuously for several minutes to induce precipitation. Isolate the precipitatc by vacuum filtration. Rinse the product with a couple mL of cold acetone. Dry the product on the vacuum for 10 minutes. Obtain the final mass of your product & an IR spectrum. Submit a sample for 'H NMR spectroscopic analysis in DMSO-d. Data Table - Preparation of a-chloro-2,6-dimethylacetanilide Mass of 2,6-dimethylaniline used 2.500 Volume of a-chloroacetyl chloride 2.000 Volume of glacial acetic acid 20 Mass of product obtained 1.567 Percent yield 47.6% Data Table - Preparation of Lidocaine Mass of a-chloro-2,6-dimethylacetanilide used 1.249 Volume of diethylamine 3.4 Mass of Lidocaine obtained 3.868 Percent yield १०.१२ Data Table - Preparation of the bisulfate salt of Lidocaine Mass of Lidocaine used 1.673 Volume of 2.2 M H2SO4 used 2.00 Mass of the bisulfate salt of Lidocaine 0.872 Percent yield 53.26 8 8 ml 8 ml B ml
Calculate the overall percent yield for the four-step synthesis • Given the yields that you obtained in this synthesis, calculate the number of moles of 2,6- dimethylnitrobenzene that would be needed to prepare one mole of bisulfate salt of lidocaine.