Hydrazine hydrate (0.25 mol, 2.5 equiv) was added dropwise to a solution of 4,6 dichloro pyrimidine 3,6 dichloro pyridazine ( 0.1 mol, 1 equiv) in ethanol (100 mL) for 30 oC at room temperature. After stirring at 30 oC for one hour, dump the reaction mixture after one hour creamy precipitated appears. Filter the product (78% yields), use the crude product for next step synthesis.
The purpose of this experiment was to determine the formula of a hydrate CuSO4 specifically, determine the amount of water in that hydrate. In order to do so, a sample of the hydrate was placed in a crucible that sat above a flame. The flame, provided by a Bunsen burner, aided in the evaporation of the water existing in the hydrate. By recording the mass of the hydrate sample before and after it was heated, the water lost due to evaporation could be calculated; 5 molecules of H2O was concluded. This information allowed the formula of the hydrate to be determined: CuSO4 • 5H2O(s)
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
Experimental Method: A filtration apparatus was set up. Solid iron(III) chloride hexahydrate was dissolved in water. In a separate container, sodium acetate trihydrate (NaC2H3O2 x 3 H2O) was also dissolved in water. Sodium acetate trihydrate was then added to iron(III) chloride. 2, 4-pentanedione (C5H8O2) was dissolved in methanol; it was then added to the iron(III) chloride/sodium acetate solution. The product of this mixture was filtered, and the precipitate
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
The goal of this was to successfully accomplish the synthesis of para-Chlorophenoxyacetic acid. In this experiment, para-Chlorophenoxyacetic acid was synthesized from 4-chlorophenolate and chloroacetic acid using an SN2 reaction. The product obtained was determined to be the para isomer of Chlorophenoxyacetic acid. This was confirmed by the melting point of 157.3-157.9 ◦C. The percent yield determined at the end of the experiment was 37.83 %. The TLC analysis showed that P-Chlorophenol was less polar than P-Chlorophenoxyacetic Acid because it had an Rf value of 0.38 in comparison to the value of 0.33 on a 50:50 hexane and ethyl acetate solvent mixture. In the NMR comparison, it was shown that both the starting material of chloroacetic acid and product contained a peak of integration two around 4 ppm representing the acidic proton. In the FT-IR comparison, it was determined that the Chloroacetic acid and the para-Chlorophenoxyacetic acid both had an OH bond at 3416 cm-1 and 3429.72 cm-1 respectively. The Chloroacetic acid and para-Chlorophenoxyacetic acid also both had a carbon-oxygen double bond at 1648 cm-1 and 1654.81 cm-1 respectively. The para-Chlorophenoxyacetic acid also contained a peak at 1236.18 cm-1 which represents the C-O-C bond.
To start off, in an Erlenmeyer flask approximately 0.51 g of E-stilbene with 10 mL of acetic acid was dissolved. A hot water bath was prepared and the mixture was warmed until the solid is completely dissolved. After the solution was dissolved, 1.02 gram of pyridinium hydromide perbromide was added. The crystals around the flask were rinsed with a small amount of acetic acid and the solution was continued in the hot water bath for one to two minutes.
In this lab, "Gravimetric Methods," students were expected to be able to calculate the mass percentage of an unknown hydrate, describe the process of gravimetric analysis, and put together the equipment needed to evaporate water from the unknown hydrate. Gravimetric analysis is the process in which an amount of a substance can be found by measuring the mass. By comparing the masses of two compounds that contain the substance, one can successfully complete a gravimetric analysis. The initial recorded mass will be different from the final recorded mass since part of the substance evaporates from the container. By subtracting the initial mass from the final mass, students can determine the amount of the substance that evaporated. They can
Reaction 1 involved a primary alcohol (OH), weak leaving group in the starting material and a reaction with a strong nucleophile (sodium bromide) and a polar protic solvent (sulfuric acid). The reaction was carried out through reflux and the product had a relatively high yield (75%) (Scheme 1).
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)
Procedure: Preparation of solution of unknown hydrate: 1. A clean dried test was taken. 2. A sample of unknown hydrate was taken in test tube.
To a 5 mL conical vial with a spin vane, 5-nitro-2, 3-dihydrophthalazine-1, 4-dione (.151 grams) was added. Next, sodium hydroxide (2 mL, 3M) was added to the conical vial and stirred until a reddish brown color was obtained. The addition of sodium hydrosulfite (.254 grams) followed, and the sides of the conical vial were
Hydrazine is a corrosive and highly toxic chemical propellant. At room temperature, Hydrazine has high vapor pressure which causes a natural movement of propellant for the combustion task. While the studies from decades indicate that the chemical propellants are superior in achieving efficient performance, they also raise a great level of environmental concerns. Ground impacts, Atmospheric impacts, Space impacts and biological impacts are four important areas which are observed to be highly affected. Mishandling the highly toxic hydrazine can result in explosions and fatal accidents. Periodic explosions were observed when the propellant exhaust gets in touch with the atmosphere. Space based impacts are considered as there are noticeable effects of debris in space.
Another candidate is N2H4BH3 (hydrazine borane, HB) solid with 15.4 wt% hydrogen capacity, which can release 5.8 wt% H2 at 140 C in 12 min [4] and can yield 11 wt% H2 at 150 °C in less than an hour after mixing with LiH, has attracted more attention and has been experimentally studied as one novel B-N-based material for hydrogen storage through different routes, such as thermal decomposition, hydrolysis, etc… [5-9]. This material can be easily prepared from a reaction of dihydrazine sulfate with sodium borohydride [4].
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.
Subsequently, 10mL of 3.5% H2O2 were added dropwise to the reaction mixture and was stirred for 20 minutes before heating to boiling at 80°C for 5 minutes. The reaction mixture was then taken off heat and allowed to cool undisturbed in an ice-bath for 30 minutes. Suction filtration was performed after to collect the crystals from the chilled solution The product was then washed with chilled 95% ethanol (2 x 15mL) and followed by diethyl ether (2 x 10mL). The crude product was then left to dry before recording the yield. 20mg of the crude product is then accurately weighed out and dissolved in deionized water in a 25mL volumetric flask. Deionized water was added to the volumetric flask to the mark and the UV-vis absorption spectrum of the crude product was recorded.