Synthesis of t-Pentyl Chloride Introduction: 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. Results and Discussion: Main reaction(s) and Mechanism(s): Reaction: Mechanism: Table of Reactants and …show more content…
Once inverted, built-up gas was released by turning the stopcock to its opened and closed positions. This was repeated for about four times in one minute intervals. Then the layers were allowed to settle until a separation between liquids could be observed. Due to the low density of the product, the top layer was to be extracted. The bottom layer was carefully and slowly extracted out of the separatory funnel. The crude product was washed by taking the reaction product in the separatory funnel and adding 23 mL of deionized H2O. The mixture was shaken and allowed to settle until layers were observable. The top layer was the desired product and approximately 25 mL of aqueous layer was extracted from the separatory funnel. Next, 25 mL of 5% NaHCO3 was added to the separatory funnel in order to neutralize the acid. This mixture was swirled, plugged with the stopper and inverted. Built-up gas was released by turning the stopcock to its opened and closed positions, releasing CO2 by-product. This was done four times in one minute intervals. The solution was allowed to settle until layers were observable. The bottom layer that contained salt, base and water was extracted from the separatory funnel. The crude product was washed again as mentioned previously. The wet, crude product was placed into the 50 mL Erlenmeyer flask. Small amounts of CaCl2 were added to dry the solution. The flask was sealed and the mixture was swirled and left to settle. Once
All standardizations are performed in triplicate. Weigh out .1000-.1200 gram KIO3. Add 70-80 mL of deionized water. Swirl and dissolve. Add 3 mL of 6M HCl. Swirl and mix. Quickly titrated the brow-red solution with 0.1M Na2S2O3 until it is light yellow. Then add 3.5 mL of starch indicator. Titrate again until the dark color first disappears.
14 mL of 9 M H2SO4 was added to the separatory funnel and the mixture was shaken. The layers were given a small amount of time to separate. The remaining n-butyl alcohol was extracted by the H2SO4 solution therefore, there was only one organic top layer. The lower aqueous layer was drained and discarded. 14 mL of H2O was added to the separatory funnel. A stopper was placed on the separatory funnel and it was shaken while being vented occasionally. The layers separated and the lower layer which contained the n-butyl bromide was drained into a smaller beaker. The aqueous layer was then discarded after ensuring that the correct layer had been saved by completing the "water drop test" (adding a drop of water to the drained liquid and if the water dissolves, it confirms that it is an aqueous layer). The alkyl halide was then returned to the separatory funnel. 14 mL of saturated aqeous sodium bicarbonate was added a little at a time while the separatory funnel was being swirled. A stopper was placed on the funnel and it was shaken for 1 minute while being vented frequently to relieve any pressure that was being produced. The lower alkyl halide layer was drained into a dry Erlenmeyer flask and 1.0 g of anhydrous calcium chloride was added to dry the solution. A stopper was placed on the Erlenmeyer flask and the contents were swirled until the liquid was clear. For the distillation
The mixture was heated at 120°C using an aluminum block and was stirred gently. After all of the solid dissolved, it was heated for 20 additional minutes to ensure the reaction was complete.
1. Carefully measure the volume of the trapped gas using the graduations (markings) on the side of the container.
In this experiment, a mixture of unknown #3 was used. That mixture had acid, base, and neutral. We added solvent to the unknown. It is important to know the density of the solvent in order to determine which is the aqueous layer and which is the organic layer. If the solvent that has more density than water, so the organic layer will be the lower layer, while if the solvent has lower density than water, the organic layer will be the upper layer. This will make an error if the determination of the layers was wrong after added the strong acid or the strong base. We added 5% HCl to the mixture in order to separate the base in the aqueous layer and form its salt. Same thing, we add 5% NaOH to the mixture in order to separate the acid and form its salt. In order to recover the base, we add 10% NaOH to the HCl extraction. The result will be salt with a base. Same thing for the acid, in order to recovered it, we added 10% HCl. The reaction will give us salt with an acid. For the neutral, we added sodium sulfate as a drying reagent in order to dry water and separate the neutral part as pure.
The purpose of this experiment was to synthesize t-pentyl chloride from the reaction of t-pentyl alcohol and concentrated HCl. This reaction occurred through an SN1 reaction, a unimolecular nucleophilic substitution reaction. This was a First Order Rate Reaction where the rate of t-pentyl chloride was dependent only on the concentration of t-pentyl alcohol. After the reaction was completed, the products were achieved via 3 liquid-liquid extractions and then after by simple distillation. In the liquid- liquid extractions a solute was transferred from one solvent to another. Then in the simple distillation the miscible liquids or the solution, was separated by differences in boiling points. After this the product was determined through infrared spectroscopy.
9.Repeat the procedure with a new mass of baking soda. Before beginning, rinse the reaction vessel with water. Refill the graduated cylinder with water. Check water level in collection box so it has room for the water from the graduated cylinder.
Wash (swirl and shake) the organic layer with one 10-mL portion of water and again drain the lower aqueous layer. Transfer the organic layer to a small, dry Erlenmeyer flask by pouring it from the top of the separatory funnel. Dry the crude t-pentyl chloride over 1.01 g of anhydrous calcium chloride until it is clear (see Technique 12, Section 12.9). Swirl the alkyl halide with the drying agent to aid the drying.
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)
1.) Transfer the distillate to separatory funnel. Fluid didn’t seem very clear but sufficient to finish our lab on time.
In the separating funnel, a heterogeneous mixture was formed: resulting in an organic layer (top) and a solvent layer (bottom). This effectively allowed the draining of the solvent, in order to isolate the organic layer, the impure ester (1-pentyl ethanoate)
Chlorine is used for many useful purposes in the world of medicine. For this reason, it is important to understand what chlorine is and how it works at the atomic level. The first notable piece of information taken from Figure 1 is the shells of the model. Each shell can be thought of as an orbit around an atom's nucleus. The shells, from the inside out, are labeled as the 1 shell, 2 shell and 3 shell. They can also be called K shell, L shell and M shell, respectively. The first most important piece of information taken from Figure 1 are the shells. Each shell has a fixed number of electrons that it can hold. 1 shell can hold up to two electrons, 2 shell can hold up to eight electrons and 3 shell can hold up to 18 electrons. The number of shells
If necessary the centrifuge can also be used to further separate the two layers. A final means of drying the ester product is the addition of granular sodium sulfate.
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.
The black precipitate was allowed to settle and then the supernatant, the clear liquid that lies above a precipitate, was decanted, or poured carefully off. Then, 200 mL of hot distilled water was added and the precipitate was allowed to settle to repeat the decanting process again.