Monomer And End Capper Synthesis Lab Report

Initially, the entire impure product was mixed with diethyl ether for extraction. Upon mixing, the solution separates into two layers; an organic layer and an aqueous layer. The organic layer contains the desired product. Additional extractions using sodium carbonate solution and sodium hydroxide solution were used as well to ensure removal of undesired molecules. The reason that two layers form is due to the fact that water is immiscible with organic products and diethyl ether meaning that they do not dissolve into one another.

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)

2-Methycyclohexanol (15mL) were added to H3PO4 (1mL) and H2SO4 (3 drops) in a 100mL round bottom flask. The distillation apparatus was assembled and the mixture was moderately heated to avoid bubbling during the distillation process. During this time, some of the equipment was not 100% secured, and some product was lost. Distillation was stopped when a black, oily substance started to form at the bottom of the flask. The distillate was collected in the Erlenmeyer flask, at the temperature of 109 degrees C. The organic layer was dried using the anhydrous MgSO4. The MgSO4 was filter off and the alkene mixture was collected. The liquid alkene was weigh.

To proceed in the reaction Bromine, reddish-brown, solution is added into a solution of the cholesterol and MTBE solution. After that is done, the solution is mixed by swirling the flask around until getting a persistent light yellow colored solution, if not retrieved more Bromine should be added. This solution is then cooled to form crystals, while the solution cools a wash solution was made to wash the solution of cholesterol bromine when being filtered. This wash is made of 1.4 mL HOAc (glacial acetic acid), and 2 mL of methyl tert-butyl ether. When the solution is cooled it is to be filtered by vacuuming, when pouring the solution into the funnel, the reaction vial was washed with the wash solution that was made. This is done to make sure you are recovering all of the crystals in your solution. When the vacuuming is all set the crystals were left out to dry for a week and the mass and melting point were retrieved.

Synthesis of tetrakis (pyrrolidino) phosphonium tetrafluoroborate (Py4P1+BF4-), tetrakis (piperidino) phosphonium tetrafluoroborate (Pi4P1+BF4-), and tetrakis (morpholino) phosphonium tetrafluoroborate (Mo4P1+BF4-).

The objective of Part 1 of this experimental procedure includes the isolation of a pure trimyristin from the mixture of compounds in nutmeg. The objective of Part 2 of this experimental procedure includes synthesizing myristic acid from the previously produced and collected trimyristin by hydrolysis. The myristic acid in its crude form will be recrystallized for purity. All products and compounds will then be tested for purity by taking their melting points.

Then 0.5 mL of bromobenzene was slowly added dropwise through the top of the condenser. The reaction was then stirred for 15 minutes. The reaction was poured into a small beaker containing 5 mL of water. Then the solid product was filtered and washed with a few milliliters of water. Lastly, the solid

1H and 13C NMR spectra were taken on a 400 MHz NMR spectrometer and CDCl3 was used as solvent. Chemical shifts are reported in parts per million shift (δ-value) from (CDCl3) (δ 7.24 ppm for 1H) or based on the middle peak of the solvent (CDCl3) (δ 77.00 ppm for 13C NMR) as an internal standard. Signal patterns are indicated as s, singlet; d, doublet; dd, double doublet; t, triplet; m, multiplet; bs, broad singlet; bm, broad multiplet. Coupling constants (J) are given in hertz (Hz).

Ultimately, the aqueous layer was washed away and the ether layer containing the desired product was left. The brine solution was added and acted as a pre-drying agent, where it extracted the water out of the organic layer. In molecular terms, the water is attracted to the ionic brine solution and thus drawn out into the aqueous layer. The addition of anhydrous sulfate dried the solution more and gravity filtration was performed to obtain the final products of 1-ethoxybutane and ether.

The HDI/PCN/BD stoichiometric ratio for the synthesis of the final polymer was kept as 4:3:1. The polymer solution was passed through a Teflon filter in order to

As the distillate was obtained from the steam distillation, several liquid-liquid extractions with methylene chloride were performed in separatory funnels to separate the aqueous water layer from the organic layer. The formation of two distinct layers occurred because the two liquids are immiscible and will not mix together because of their solubility and density differences. The organic methylene chloride layer formed the bottom layer, because it is more dense than water forcing the aqueous water layer to the top. The organic layer at the bottom was dispensed into a flask, leaving the aqueous layer in the funnel to perform two additional washes. The next extractions were done using ether and the remaining organic layer liquid from the flask. Ether is less dense than water so the organic ether layer formed the top layer and the aqueous layer formed at the bottom.

The solution was poured into a 125ml separatory funnel and was extracted with three portions of 20:80 ethyl: hexanes. The organic layer (the top one) was obtained and all the organic layers were combined. The layers were washed with saturated sodium chloride in the separatory funnel. The organic solution was dried using magnesium sulfate anhydrous. The organic solution was the filtered. The

The mixture was stirred for 2 h at room temperature. The reaction mixture was stirred at the same conditions (–10◦C) for 2 h, and then the mixture was allowed to warm up to room temperature and was stirred for 4 days. The solvent was removed under reduced pressure and the viscous residue was purified by flash column chromatography (silica gel powder; petroleum ether–ethyl acetate, 10:1). The solvent was removed under reduced pressure and the product 4 was obtained. The characterization

The mixture was heated to a gentle boil and then the distillation was allowed to begin. The heat was turned off after the temperature of the steam stayed constant. The distillation continued until approximately 40 mL of the liquid was obtained. The 40 mL of distillate was transferred to a 250 mL separatory funnel. A small amount of dichloromethane was used to wash the receiver after the transferal. The distillate was extracted with 10 mL of dichloromethane three times, each time using a little extra dichlormethane to wash each layer. The organic layer on the bottom was collected for each extraction. All organic layers were collected in a 125 mL Erlenmeyer flask. Anhydrous sodium sulfate was used to dry the solution for fifteen minutes. Meanwhile, a vacuum filtration apparatus was set up accordingly. A 250 mL filter flask was obtained and pre-weighed. The solution containing the limonene was vacuum filtrated while it was kept warm in a steam bath. Additional Sodium Sulfate was added to the solution to remove excess water. The solution was then washed 3-4 times with dichloromethane and the vacuum filtration continued. The vacuum pump was turned off when the flask contained only a small amount of oil. The flask was then weighed.

The purpose of this lab was to investigate the method of extraction as a means of isolating pure compounds. In this experiment, the acid-base extraction method was used on a mixture composed of three separate components: an acid, a base, and a neutral component. The extraction solvent used was diethyl ether. Through sequential acid-base reactions where aqueous 10% NaOH and aqueous 10% HCl were used in a separatory funnel, the three components were extracted, isolated and then recovered through precipitate reverse reactions using 10% NaOH and concentrated HCl. Once the components were isolated and recovered, a melting point analysis was performed and these values were then compared to the values in the laboratory handout in order to identify the compounds. Percent yield of each compound was also calculated. It was found that the mixture contained Benzoic Acid with a melting range of 121.6-122.9 oC and a percent yield of 292%, Meta-nitraniline with a melting range of 111.4-112.2 oC and a percent yield of 204%, and Biphenyl with a melting range of 70.6-73.5 oC with a percent yield of 128%.