Hcl Synthesis Lab

Reaction 2 - 1.Used a Beral- type pipet, added about 2mL (40 Drops) of 1M hydrochloric acid solution to a small test tube.

3. Under a fume hood, drops of concentrated HCl(aq) were added to each test tube.

The first step that needed to be done in this experiment was adding hydrochloric acid (HCl)

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.

3.0g of salicylic acid was weighed then 3.0mL of acetic anhydride and 6 drops of 85% H3PO4 were added to it. The mixture was warmed over a water bath for 5 minutes while stirring. After warming, 20 drops of distilled water was slowly added. 15mL of water was added then the solution was heated until it became clear. It was allowed to cool and was placed in an ice bath until the solution becomes cloudy. Using pre-weighed filter paper, the mixture was filtered and was allowed to dry in the filter paper.

The makeup of a compound drastically changes its intermolecular forces (IMFs) with the polar silica gel of a TLC plate; this concept is responsible for the variability of Rf values observed throughout the course of lab. The weaker the IMFs, the further a compound will travel through the silica. For instance, ionic interactions are the strongest IMF, but were not present during this experiment. H-bonding IMFs had the greatest impact for our specific compounds. Resorcinol and 3-chlorobenzoic acid exhibited low Rf values, due to its ability to H-Bond to silica’s hydrogen donors and oxygens acceptors (See graph 1). Both were adept to strongly H-bonded to silica because the compounds contained at least 1 H-donor and 2 H-acceptors. Thus, stronger/more

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.

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.

In a 25-mL round-bottom flask, 1-chlorobutane (5 mL, 4.32 g, 0.046 mol), sulfuryl chloride (1.6 mL, 2.7 g, 0.02 mol), 2,2’-azobis-(2-methylpropionitrile) (0.03 g), and a boiling chip were added. After a condenser and gas trap were attached to the flask, the mixture was heated to a gentle reflux in a steam bath for 20 min. The flask was then allowed to cool down quickly in an ice bath for a short time before a second portion of the 2,2’-azobis-(2-methylpropionitrile) (0.03 g) was added to the flask. The mixture was refluxed for another 10 min. before the flask was cooled in a beaker of water. The reaction mixture was then poured into a small separatory funnel already filled with water (10 mL),

After dissolving benzoic acid in 1.0mL CH2Cl2 and 1.0mL 10% NaHCO3 solution, two layers are created, the top layer is 10% NaHCO3 solution and the bottom is CH2Cl2.

2) Rinse the solid with about 30 mL of distilled water and decant the liquid from the solid. It is critical that as little solid as possible is lost during this process. Repeat the rinsing two or three times.

5.3 mL of bromobenzne and 15 mL of anhydrous ether was then placed into the separatory funnel and was shaken and vented in order to mix the solution. Half of the bromobenzene solution was added first into the round bottom flask and as soon as a color change was observed, the remaining half of the bromobenzene was added drop wise into the round bottom flask. The mixture was then refluxed on a heating mantle for 10 minutes until most of the magnesium has been consumed.

This process was then repeated two more times with subsequent additions of 10 mL of the 0.5M aqueous NaHCO3 and the aqueous layers drained off into the above mention labeled 100-mL beaker. Finally 5 mL of deionized water was placed into the funnel and mixed. The water was then drained off into the beaker containing the aqueous solution extracts. The solution was then saved until need later in the experiment.

Five 250mL Erlenmeyer flasks were obtained. Then, 200mL of hydrochloric acid (HCl) was poured into a 600mL beaker. The gelusil

Step 1 and 2 was repeated by using distilled water by replacing the test solution.