Lab Report Chemistry Lab
Since the Grignard reagent can easily react with water, all glassware including the 25 ml round bottom flask, magnetic stir bar, 3 and 5 ml conical vial, 50 mL Erlenmeyer flask, claisen adapter, drying tube and 5 glass pasteur pipets were first added to a 250mL beaker and placed in the oven for 30 minutes. After the completion of the thirty minutes, 0.150 g of shiny magnesium turnings and a stir bar was first added to the round bottom flask and the claisen adapter along with the drying tube packed with calcium chloride was added to one of the heads of the claisen adapter. A rubber septum was then added to the other head and the entire apparatus is placed on a hot plate at its lowest setting. Meanwhile, 20 ml of anhydrous diethyl ether was added to a 50 ml Erlenmeyer flask and sealed using a rubber septum.
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Then, 0.7 ml of bromobenzene was added to a pre-weighed 5ml conical vial and the starting mass was measured.
A pasteur pipet was then used to transfer 4ml of anhydrous ether to the vial. The syringe was then utilized to transfer 0.8 ml of this solution and the reaction was allowed to proceed until the solution turns brown and cloudy. The conical vial was then rinsed with 2 ml of anhydrous ether to get any remaining solution into the reaction vessel. Simultaneously, 1.09 g of benzophenone and 2ml of anhydrous ether were added to a 3ml conical vial and gently stirred. The reaction vessel was taken off of the hot plate and allowed to cool. The benzophenone was then added to the reaction mixture while stirring vigorously. The conical vial was washed with anhydrous ether and transferred to the mixture. The reaction mixture is then transferred into a beaker and stored in a drawer after 15 minutes until next
lab. At the starting of the next lab 6ml of 6M HCl was first added to the beaker and a glass rod was used to break any solids. Then, 10 ml of diethyl ether was then added to the beaker and mixed until two layers were formed. The solution was then added to the separatory funnel was the clamped funnel was shaken while pointing the funnel upward to prevent any leakage. The stopcock was released every now and then to release any pressure and clamped once again before shaking the funnel. The funnel was washed with diethyl ether twice and the aqueous layer was removed each time. The final remaining organic layer was then transferred into an Erlenmeyer flask and sodium sulfate was used to dry out any remaining impurities and the final organic layer was transferred to a 30 ml beaker and washed with diethyl ether twice and decanted each time. Then, 7ml of petroleum ether was added to the beaker containing the dried organic layer and then slowly heated to evaporate the solvent. The beaker was then covered using in an aluminum foil and placed in an ice bath until crystals were formed. The filters were then filtered using a Hirsch funnel and vaccum filtration. The funnel was also washed using 2ml of petroleum ether twice and allowed to slowly filter. The dried crude product was then weighed before adding isopropyl alcohol. Once the isopropyl alcohol was used to dry the product the beaker was covered using a foil and placed in an ice until more crystals were formed and then filtered out once again using a Hirsch funnel and vacuum filtration. The final product was then filtered out once again and melting point analysis and an IR spectroscopy were conducted to characterize the product [1].
Then, 0.7 ml of bromobenzene was added to a pre-weighed 5ml conical vial and the starting mass was measured.
A pasteur pipet was then used to transfer 4ml of anhydrous ether to the vial. The syringe was then utilized to transfer 0.8 ml of this solution and the reaction was allowed to proceed until the solution turns brown and cloudy. The conical vial was then rinsed with 2 ml of anhydrous ether to get any remaining solution into the reaction vessel. Simultaneously, 1.09 g of benzophenone and 2ml of anhydrous ether were added to a 3ml conical vial and gently stirred. The reaction vessel was taken off of the hot plate and allowed to cool. The benzophenone was then added to the reaction mixture while stirring vigorously. The conical vial was washed with anhydrous ether and transferred to the mixture. The reaction mixture is then transferred into a beaker and stored in a drawer after 15 minutes until next
lab. At the starting of the next lab 6ml of 6M HCl was first added to the beaker and a glass rod was used to break any solids. Then, 10 ml of diethyl ether was then added to the beaker and mixed until two layers were formed. The solution was then added to the separatory funnel was the clamped funnel was shaken while pointing the funnel upward to prevent any leakage. The stopcock was released every now and then to release any pressure and clamped once again before shaking the funnel. The funnel was washed with diethyl ether twice and the aqueous layer was removed each time. The final remaining organic layer was then transferred into an Erlenmeyer flask and sodium sulfate was used to dry out any remaining impurities and the final organic layer was transferred to a 30 ml beaker and washed with diethyl ether twice and decanted each time. Then, 7ml of petroleum ether was added to the beaker containing the dried organic layer and then slowly heated to evaporate the solvent. The beaker was then covered using in an aluminum foil and placed in an ice bath until crystals were formed. The filters were then filtered using a Hirsch funnel and vaccum filtration. The funnel was also washed using 2ml of petroleum ether twice and allowed to slowly filter. The dried crude product was then weighed before adding isopropyl alcohol. Once the isopropyl alcohol was used to dry the product the beaker was covered using a foil and placed in an ice until more crystals were formed and then filtered out once again using a Hirsch funnel and vacuum filtration. The final product was then filtered out once again and melting point analysis and an IR spectroscopy were conducted to characterize the product [1].