Before the start of the experiment, the theoretical yield was to be calculated. First, the limiting reagent was determined from the reagents by comparing the amount of moles. Among the three reagents involved in this experiment - camphor, sodium borohydride, and methanol, camphor was found to be the limiting reagent. The moles of camphor was less than the combined moles of the other two reagents. The theoretical yield, which is the amount of product that could be possibly produced after the completion of a reaction (“Calculating Theoretical and Percent Yield”), was found to be 0.25 g. Once the product was achieved, a percent yield of 97% was determined. As a result, the reduction of camphor to isoborneol was successful. In order to achieve isoborneol from camphor, a mixture of camphor with methanol and sodium borohydride was heated for about two minutes. Data Table 1 demonstrates the measurements that were taken to prepare the reaction mixture. The addition of sodium borohydride caused the reaction to fizzed. …show more content…
The result was small white crystals, which were dry and had barely contained any moisture. The product was then dissolved in methylene chloride and dried with granular anhydrous sodium sulfate. The drying agent would have removed any water in the solution and presented a colorless solution. The solvent was evaporated and the product was collected; it had the appearance of small, white solids. Data Table 2 shows the results and calculations that were gathered after the completion of this experiment. A boiling point of the product was found to be 210℃. According to literature, the boiling of isoborneol should be 212℃. As a result, the product is most likely isoborneol. No errors had occurred during the course of the experiment, which is testified by the high yield of
0.98 grams of Camphor was dissolved in 15 mL of ethanol. 1.055 grams of sodium borohydride was added was slowly added to the mixture. The mixture was left standing for ten minutes then it was heated to boiling. 5.00 mL of ethanol was added to keep the volume during the hot water bath. The mixture was then poured into 100mL of ice water. A white precipitant was formed immediately. The solid was recrystallized in a water and ethanol solution. 1.65 grams of product was measured after filtration and drying. 1mL of the counter-solvent, water, was added to the
A & C: MEASURING THE OPTICAL ROTATION OF CAMPHOR SAMPLES AND CAMPHOR OBTAINED FROM OXIDATION OF ISOBORNEOL
The purpose of this experiment was to perform a reduction reaction using camphor in methanol with sodium borohydride. This reaction generated a mixture of diasteroemers; bornoel and isoborneol. NMR analysis was used to determine the product ratio of isoborneol to borneol. In this experiment, 100 mg of camphor, appearing as white crystals, were dissolve in 1 mL methanol. Four portions of approximately 25 mg of sodium borohydride were added.
16 (Scheme 6) was purified by column chromatography (10% MeOH/DCM). The product, however, came too quickly off the column and wasn’t purified enough. A second column (1% MeOH/ DCM) was done to purify it further. The yield was 46%.
In the figure above showed the mechanism of synthesizing methyl eugenol from eugenol. In order to successfully synthesize methyl eugenol, the eugenol went under an SN2 reaction where the potassium carbonate and the tetrabutylammonium bromide deprotonated the phenolic group of the eugenol. Once the phenolic group deprotonated, the conjugate base of eugenol attacks the dimethyl carbonate and that caused a substitution reaction with methyl carbonate, creating methyl eugenol. The mechanism regarding the synthesis of 2-allyl-4,5-dimethoxyphenol and trans-coniferyl alcohol (sex pheromones) was made due to the breakdown of methyl eugenol (pheromone precursor) through bacteria dorsalis enzymes.
2,3- Dimethyl- 2,3-butanediol weighed 1.20g, it was added to a 10 ml round bottom flask filled with 4 ml of sulfuric acid. This entire reaction was put into a simple distillation to be heated and distilled into a vial then collected when the mixture reached around 100 degrees celsius. Once the product was collected, the aqueous layer was removed and a total of 2 ml of saturated NaCl was added in order for the product to be washed. The organic layer was placed back in the vial to dry with sodium sulfate that weighed 0.724g of clear liquid. The final product was purified by distillation and started to collect at 100 degrees celsius and before the distillation ended the temperature increased to 104 degrees celsius. Which led the weight of the
Isobutyrophenone was weighted out into a 150ml beaker, methanol and a stir bar was added as well. The solution was stirred and sodium borohydride was slowly added—after it was added, the solution was allowed to stir for approximately 20 minutes. After stirring, hydrochloric acid was added to the methanol solution—the solution was placed in the fume hood.
Methanol, or wood alcohol (CH3OH), could be a predominant solvent for chemical industrially, it's a wonderful solvent with sensible capability and physical properties like low melting point, that makes it a decent refrigerant, and it's thought-about and utilised as immaculate artificial fuel. The chemical identity of alcohol was established within the nineteenth century, and therefore the 1st business plant for the alcohol synthesis was designed by BASF in 1923. the method concerned alcohol synthesis from synthesis gas utilizing a Cr chemical compound /zinc chemical compound catalyst at temperature of 300 °C and pressure of 200 atm. This method is nonetheless kenned as aggressive synthesis of alcohol (CH3OH) (Sunggyu 1990).The numbers of amendments
A test tube was acquired, and 7 mL of concentrated HCl were added to this test tube through a graduated cylinder, this was done in the fume hood in order to avoid any noxious fumes from the sample, which were observed when pouring in the concentrated HCl. After adding the HCl, a glass pipet was used to add 2.5 mL of tert-butyl alcohol to the test tube. It was observed that the alcohol and HCl separated into two layers distinct layers. The solution was mixed by using the pipet to take the bottom layer and squirt it onto the top, this mixing process was performed for 15 minutes to allow the solutions to mix well. Afterwards, the lower aqueous layer of the test tube was removed with the pipet; it was imperative to remove as much of the lower layer as possible without removing too much from the top layer. The solution was then washed with water by pouring 2.5 mL of water into the test tube, letting it sit for about a minute and then removing the aqueous layer again, in order to help the mechanism for this process. Additionally, about 2.5 mL of sodium bicarbonate 5% were also added to he test tube, were allowed to sit for about a minute, and then removed once again; this was done in order to remove any HCl impurities from the solution. The remaining upper layer was moved to
To begin, we observed the physical properties of our substance. Physical properties include smell, physical appearance, odor, and color, as well as any other properties that can help identify a substance simply from observation. We noticed fairly large, white granules that didn’t have a great tendency to stick to one another. These results can be viewed in Table 1. There was no noticeable odor to our compound, or any other visible identifiers. Sodium Chloride is an odorless, colorless solid that dissolves completely in water. Our results matched these properties.
The calculation of theoretical yield is required for this investigation. Theoretical yield is the amount of product synthesised from a successfully completed chemical reaction. It is calculated from the stoichiometry of the initial reaction, and thus
The reason for this experiment was to conduct a benzophenone reduction using sodium borohydride in order to synthesize diphenylmethanol.
This report describes the attempt at preparing cyclohexene via a dehydration reaction of cyclohexanol. The reaction must proceed under acidic conditions for the alcohol group on the starting material to become protonated; if not protonated, it is a bad leaving group, but once it has been protonated to become -H2O+, it can readily depart. After this step, a base must be present to complete the elimination reaction by removing a proton from the carbocation intermediate and thus enacting the formation of a double bond. This base must be a bad nucleophile so that a substitution reaction instead of the desired elimination does not take place, and it should be strong enough to accomplish this step. The first criteria can be taken care of by using H2SO4 as the acid that protonates the leaving group, as HSO4- is a poor nucleophile, especially as compared to the conjugate base of HCl which was used to accomplish the substitution reaction earlier this semester; however it is also a weak base, so water must be included in the reaction to accomplish the elimination, as it is much more effective at deprotonating the carbocation.
The chemicals methanol and water (pH between 5 and 8) were HPLC grade and were purchased from Merck chemicals private limited, Mumbai. Sodium acetate and acetic acid used in this work were analytical grade purchased from Merck chemicals,
Oil used were lauric oil, vegetable oil and lard. Each triacylglycerol was weighed to 1.0g. Each were placed n separate round bottom flask.. 15mL of 5% alcoholic KOH was added into each flask from a burette. KOH was used in order to hydrolyze the glyceryl esters to glycerol and the potassium salts of fatty acids. Alcoholic KOH was used to allow oil be soluble in it. [1] Two to three pieces of boiling chips were added so as to prevent formation of large bubbles [1]. It was then subjected to reflux for an hour. After which, it was then cooled to room temperature. The solution was then transferred into an Erlenmeyer flask. Small amounts of hexane were added to rinse of remaining oil from the round bottom flask. It was then titrated with 0.5M HCl, using 1% phenolphthalein as the indicator. Volume of KOH used was used to determine the saponification number by using the eq. 2