Separation Of Methanol And Narolin Crystals

The product was then suspended in 2 ml of water with a stir rod in a 50 ml Erlenmeyer flask and heated to boiling. Water was added in one milliliter increments until all the product was dissolved (18 ml added total). The saturated solution was allowed to slowly cool, and gradual white crystal formation was observed. Recrystallized product was collected once more by suction filtration with the Hirsch funnel once crystallization ceased. Collected product dried on a watch glass for a week, weighed 0.14 g (1.2 mmol), and the melting point was 139°-141°

The melting point of the final product, diphenylacetylene, was found to be 65-68 degrees Celsius which is right around the ideal 61 degrees Celsius melting point; this shows that purification during the lab worked and that the sample was almost 100% pure. Since only 0.01g of diphenylacetylene was collected and the theoretical yield was calculated to be 0.049g, this experiment had a 20.41% yield. A few sources of error that explain the low percentage could be the loss of crystals when transferred from the test tube to the suction apparatus or when they were transferred from the suction apparatus to the filter paper to be dried and then weighed. Crystals could have also been lost if more than 5 drops of methanol was added because excess methanol would dissolve the crystals. The experiment was successful when looking at the crystals collected from the addition step and the elimination step; however, to improve the percent yield and collected product the the test tubes could have been allowed to cool down in the ice bath past the 5 minutes to ensure all the crystals formed

The experiment began by mixing the initial 1.775g isopentyl alcohol with 2.3 mL acetic acid and about 5 drops sulfuric acid. This reaction mixture was then heated under reflux for an hour after boiling of the reaction mixture began.

It was made basic by adding 6 mL of 6M NaOH to the separatory funnel. The pH was taken to confirm that it was basic. Next, 10 mL of dichloromethane was added to the flask. The flask was shaken and the bottom layer was drained in a flask. This was repeated two more times. Na2SO4 was added to the flask to remove water. A flask was pre-weighed and gravity filtration was conducted. After, a TLC was conducted for p-toluidine and there was only one spot on the plate with an Rf of 0.32. Then a boiling stick was added to the flask and was placed on sand bath to completely boil. The weight of the flask was taken again.

alcohol (2-methyl-2-butanol, MW _ 88.2, d _ 0.805 g/mL) and 25 mL of concentrated hydrochloric acid (d _ 1.18 g/mL). Do not stopper the funnel. Gently swirl the mixture in the separatory funnel for about 1 minute. After this period of swirling, stopper the separatory funnel and carefully invert it. Without shaking the separatory funnel, immediately open

The product was placed in a Craig tube and several drops of hot (100°C) solvent (50% water, 50% methanol, by volume) was added and heated until all of the crystals dissolved. The Craig tube was plugged and set in an Erlenmeyer flask to cool. Crystallization was induced once the mixture was at room temperature by scratching the inner wall of the tube. It was then placed into an ice bath for ten minutes until crystallization was complete. The tube was then

After the initial mixture has refluxed, 9.11 grams of benzophenone was dissolved in 100 mL of anhydrous ether in a beaker and was then transferred into the separatory on the reflux apparatus. This solution was then added to the Grignard reagent at a drop wise rate while stirring. After the benzophenone was added, the mixture was then refluxed for 15 minutes on a heating mantle.

Methods: First, a burette, ring stand, clamp, and an empty flask were obtained. The burette, with the valve closed, was attached to the ring stand with a clamp, and the empty flask was placed below the burette. Next, 50mL of the NaOH solution were poured into the burette, and a small bit was drained into the empty flask to ensure that the tip of the burette was also full of NaOH solution. The volume of the NaOH in the burette was recorded. Next, approximately 0.6 grams of KHP were massed poured into an empty 125mL flask. Two drops of an indicator solution were added to the KHP

A 10 mL round-bottom flask was weighed both before and after approximately 1.5 mL of the given alcohol, 4-methyl-2-pentanol, was added. 3 mL of glacial acetic acid, one boiling chip, and 2-3 drops of concentrated sulfuric acid were added to the flask in that order. The reflux apparatus was assembled, the

• Filter on a Buchner funnel using a vacuum filtration for about 10 minutes. • The flask may be rinsed with the minimum amount of ice-cold acetone. • Weigh the trimyristin when dried and take a melting point. Data Weight of empty flask 48.300 g Weight of flask with crude product

An ice bath was prepared in a large beaker and a small cotton ball was obtained. 0.5 g of acetanilide, 0.9 g of NaBr, 3mL of ethanol and 2.5 mL acetic acid was measured and gathered into 50mL beakers. In a fume hood, the measured amounts of acetanilide, NaBr, ethanol and acetic acid were mixed in a 25mL Erlenmeyer flask with a stir bar. The flask was plugged with the cotton ball and placed in an ice bath on top of a stir plate. The stir feature was turned on a medium speed. 7mL of bleach was obtained and was slowly added to the stirring flask in the ice bath. Once all the bleach was added, stirring continued for another 2 minutes and then the flask was removed from the ice bath and left to warm up to room temperature. 0.8mL of saturated sodium thiosulfate solution and 0.5mL of NaOH solution were collected in small beakers. The two solutions were added to the flask at room temperature. The flask was gently stirred. Vacuum filtration was used to remove the crude product. The product was weighed and a melting point was taken. The crude product was placed into a clean 25mL Erlenmeyer flask. A large beaker with 50/50 ethanol/water

A 0.5 g of sodium tungstate dihydrate was weighed and transferred into a 50-mL round-bottom flask with a magnetic stir bar. Approximately 0.6mL of Aliquat 336 was then transferred carefully into the round bottom flask using a 1mL syringe. The round bottom flask and its contents were then set up in an oil bath. 11mL of 30% hydrogen peroxide and 0.37 g of potassium bisulphate were added to the reaction mixture in the round bottom flask and stirred using a magnetic stirrer. Lastly, 2.5mL of cyclohexene was added using automatic dispenser and the mixture stirred. A condenser was fitted on the round bottom flask, clamped and attached to water horses. The reaction mixture was then heated on the oil bath and the reflux process initiated for an hour while stirring the mixture vigorously. Half way while rinsing, any trapped cyclohexene in the condenser was rinsed. After 1 hour, the round bottom flask was rinsed

Nerolin was prepared with a mixture of methanol, 2-naphthol, potassium hydroxide (KOH), and iodoethane using a reflux apparatus. A reaction mixture was obtained, and allowed to freeze. Nerolin crystals were obtained by way of gravity filtration and vacuum filtration in a successive manner. The nerolin crystals were further analyzed to show purity of the experimental product by examining the shape and size of the crystals, along with the melting point of the crystals. From this experiment, 6.44% of nerolin crystals were recovered, with a melting point measured as 33-35C. The preparation of nerolin was performed due to its role in maintaining long-lasting fragrance release properties in fabrics.

Tube 4 now should only have crude solid in the tube and it is then weighed. The tube is placed into a 50℃ water bath and then approximately 0.5 -1 ml of methanol is added, as well as H2O until the solution gets cloudy, once the solution is dissolved it is cooled to room temperature and then iced. The crystals are then collected using a Hirsh funnel. Next a small amount (~ 0.1g) of the crystals are placed into a melting point tube and placed into the melting point machine to record the unknown neutral substances melting point.

When we tested the solubility of the starting materials, we found that all of our starting materials were soluble in hexanes, ethyl acetate, and acetone, which makes sense because all of these solutions are organic materials, so the starting materials should form London dispersion forces with them all, and the reaction should occur. Enthalpy should not care about whether the reaction occurs or not because either way it has London dispersion forces, but entropy would drive the reaction because it always wants a more random orientation, as explained above when describing enthalpy, entropy, and free energy. Interestingly, none of the starting materials were soluble in methanol. Methanol is an organic solution and contains hydrogen bonding, so