Synthesis Of 2 6-Dimethylnitrobenzene Lab Report

11) Dry out the methylene chloride solution that contain the benzoin and the dibromobenzene by the use of anhydrous sodium sulfate.

Crystallization was induced in the solution by scratching the inside of the beaker with a glass stir rod. 2. Next, an ice bath was made by partially filling a 400 mL beaker with ice and covering the ice with water. 3. The beaker containing the solution was then placed in the ice bath for approximately 15 minutes.

A spin vane was placed in the vial and the solution sat on a magnetic stir plate. The solution was stirred vigorously for 20 minutes at room temperature. After stirring it, 1 mL of diethyl either was placed with the solution and the aqueous layer was removed. The organic layer was treated with 100 mg of NaHCO3 and sat in there until the bubbling stopped. An aqueous layer formed after the bubbling and it was removed.

The colorless solution was poured into a beaker containing 10mL of chilled water, after the designated time, to initiate recrystallization for 5-10 minutes. 9. The nitrated methyl benzoate solution was then poured onto the filtrating apparatus and left to dry for 10 minutes. 10. The white, dried crystals were weighed and dissolved in ethanol then filtrated again and

To a solution of substituted chloro quinoxaline compound (2a) (4.5g, 12.9 mmol) weighed into a round bottom flask was charged with PdCl2 (dppf).DCM (6%mol, 0.633g). A toluene: ethanol mixture in 2:1 ratio (40 ml+20 mL) was degassed with nitrogen gas, and then added into the flask. Aqueous 1 molar sodium bicarbonate solution (24 mL, 19.30 mmol) was degassed and added to the mixture. The mixture was stirred at room temprature for 15 minutes under nitrogen. The 3-methyl phenyl boronic acid (2.1 g, 15.48 mmol) or respective boronic acid (2-methoxy phenyl boronic acid/ 3-methoxy phenyl boronic acid/ 2-fluoro boronic acid) was added as the solid.

The electrophilic aromatic substitution involves the uses of acetic anhydride and phosphoric acid to create the targeted product acetylferrocene. The crude product was then to be examined by thin layer chromatography (TLC). The TLC assay allows of the comparison of species based on polarity, thus showing if the reaction was successful. The crude product was then to be purified by column chromatography. The polar alumina solid phase, and mobile phase of varying polarity would allow for the separation of species found within the crude product on the basis of contrasting

The mixture was cooled to room temperature and 40mL of of water was added. The stopper was placed on the flask and shaken until the liquid residue solidified. After the product solidified, the flask was placed in an ice bath and the solid was was broken up with a string rod until it was a fine powder. The product was then collected by vacuum filtration and was washed three time with 5-mL of cold water then left to dry.

The general approach involved transforming each of the 1,3-butadienes at the site of the terminal alkene bond via reaction with the singlet oxygen. Meso-tetraphenylporphyrin was used as the photosensitiser to generate the singlet oxygen. The prepared butadienes were added to a volume of dichloromethane and cooled using a water-cooled jacketed flask. Reactions were followed by TLC and reaction times varied for each reaction based on observations. Reactions were ceased on the basis of an increasing prevalence of a new product appearing at the baseline of the TLC. Products of the reactions were purified via column chromatography. Two cycloaddition products were observed in each reaction. These were the 1,2-dioxine resulting from the Diels-Alder [4+2] cycloaddition reaction, and an aldehyde resulting from the ene cycloaddition

During week three, dissolve α-chloro-2,6-dimethylacetanilide (2.202g, 0.011mol, 3 equiv.) in toluene (30mL) and a stir bar in a dry-round bottom flask. Assemble the apparatus for heating under reflux. Then add diethylamine (2.4g, 0.033mol, 1 equiv.) to the previous solution. Then heat the mixture under reflux for 90 minutes. After the reflux is complete let mixture cool to room temperature and then ice bath for a short period of time. Then vacuum filtrate the product and rinse the solid product with toluene (5mL). Then transfer the filtrate and washing to a separatory funnel and extract it with HCl (3M, 2 x 20mL). Then combine the acidic extracts in an Erlenmeyer flask and add KOH (8M, 25mL) to make solution basic. Cool the mixture in an Ice bath. Then transfer mixture to a separatory funnel extract it with diethyl ether (2 x 15mL). Then wash the organic extracts with deionized water (25mL) and then dry it with anhydrous sodium sulfate. Gravity filtrate the solution, and cover the beaker with a watch glass till the following week. The following week weigh the product, which is pure lidocaine, determine the melting point, and perform an IR. Yield: 1.360g (0.0058 mol, 17.3%). IR (neat): 1660 cm-1 (C=O), 3252 cm-1 (N-H), 2971 cm-1

Acidity was measured again (pH = 3.5). Ice bath (10 minutes) and evoked crystallization. After crystallized fully, vacuum filtrate (5 minutes) the crystal-liquid mixture. Residue, white powder, was rinse by cold ethanol and collected.

Next add 5 g (33.80 mmoles) of phthalic anhydride and heat the mixture to 80-85° C. After 6 hours take a portion of the reaction mixture to be distilled under a vacuum, and cool to 40° C. Put 3.1 g (45.5 mmoles) of imidazole into the flask and cool it to 5-10° C. Next, cautiously drop 1.6 ml (22 mmoles) of thionyl chloride in. The mixture is stirred at room temperature for 1 hour and heated to 85° C. keep stirring at this temperature for 3 hours, then distilled to one fifth of the starting volume. The residue is then cooled to 25° C. afterwards; 100 ml of a cold ethanol mixture is added. The mixture is acidified with 37% Hydrochloric acid to the pH of 7.0—0.5. Then stir for 4 hours until it reaches room temperature. Next the precipitated solid is filtered by suction and washed twice with 25 ml of water. The resulting solid is then dried overnight under vacuum at 40° C. to give a white crystalline product of thalidomide which is 3.9 g and is a yield of

The round-bottom flask was removed from the heat and cooled to room temperature. Once the solution had cooled to room temperature, The solution was then neutralized with drops of NaHCO3 (GLR) until its pH was 7. After the solution was neutralized, the flask was put on ice so the crystals would precipitate. The crystals were then collected using vacuum filtration, rinsing with cold ethanol. The crystals were placed in a glass vial and allowed to dry for 24 hours.

In 3 mL of DMF were cooled in an ice-water bath 0.5 g (5 mmol) succinic anhydride, 0.235 g (5 mmol) of arginine ethyl ester hydrochloride was neutralized by NaOH in ethyl acetate (10 mL) and 0.5 g (5 mmol) N-methyl morpholine were added to this mixture. The reaction mixture was stirred for

Once the solution was refluxed for 5 minutes, it was then cooled for 5 minutes to room temperature with the addition of acetic acid and [acetic acid to quench (add H2)]. After the addition of acetic acid, the solution turned yellow and formed a precipitate. The solution was placed on ice for 10 minutes. Once the solution had been cooled, the solution went through a vacuum filtration until the precipitate was completely dried. The precipitate recovered is the luminol, which was used as the

Once cooled, the mixture was then transferred to a separatory funnel using the funnel while avoiding adding the boiling chip. 10 ml of water was then added to the mixture. The mixture was gently shaken and the phases were allowed to separate. The funnel was then unstopped and the lower aqueous phase was drained into a beaker. 5 ml of 5% aqueous NaHCO3 was added and then shaken gently. A great deal of caution was taken into consideration because of the production of carbon dioxide gas which caused pressure to develop inside the funnel. The pressure needed to be released so the funnel was vented frequently. The phases were allowed to separate and the lower aqueous phases was drained into the beaker. After draining, 5 ml of saturated NaCl was added to the funnel and then shaken gently. Once again, the phases were allowed to separate and the lower aqueous phase was drained into a beaker. An ester product was produced and was transferred into a 25 ml Erlenmeyer flask. This organic product was then dried over anhydrous Na2SO4 to trap small amounts of water in its crystal lattices thus removing it from the product. Finally the ester was decanted, so that the drying agent was excluded from the final product.