Experiment 1- Isolation of Trim PDF

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Brianna Galvan 13 July 2021 Experiment 1 Summer II 2021 Experiment 1: Isolation of Trimyristin from Nutmeg Introduction Medicines, insectoids, perfumes, and different beneficial natural chemical compounds may be remoted from vegetation and animals and are there're termed “ herbal products”. Trimyristin, a herbal product that may be remoted from nutmeg, belongs to a category of compounds called triacylglycerol's. Overall trimyristin must have a percentage healing of 29%. Procedure 1. Grind up nutmeg using a mortar and pestle 2. Add 15 ml of dichloromethane to the flask and set up cool to the room temperature 3. Rinse the remaining solid with 10mL of dichloromethane and filter this liquid into the beaker. Add stones to the liquid and evaporate the solvent over the plates in the fume hood. 4. Once the evaporation occurs flask the handle till cool, remove small spatula full of the crude product and set to TLC analysis. 5. Recrystallize the warm acetone that the volume of the nature solvents impacts the purity and yield of the recrystallization process. 6. Describe the melting point of the purified product SDS Trimyristin C45 H86 O6 Molecular Weight: 722.59 g/mole Powder Solid pH (1% soln/water): N/A Boiling Point: N/A Melting Point: 54 - 58 °C / 129.2 - 136.4 °F Colorless liquid. May cause eye and skin irritation. May cause respiratory and digestive tract irritation. May cause irritation of the digestive tract. May cause respiratory tract irritation. If in eyes: Flush eyes with plenty of water for at least 15 minutes, occasionally lifting the upper and lower eyelids. If gets on skin: Flush skin with plenty of water for at least 15 minutes while removing contaminated clothing and shoes. Wash clothing before reuse. If ingested: If victim is conscious and alert, give 2-4 cupful of milk or water. Never give anything by mouth to an unconscious person. If inhaled: Remove from exposure and move to fresh air immediately. If not breathing, give artificial respiration. If breathing is difficult, give oxygen.

Dichloromethane CH2Cl2 Molecular Weight: 84.93 g/mole Liquid pH (1% soln/water): N/A Boiling Point: 40 deg C Melting Point: -97 deg C Colorless liquid. Harmful if swallowed. Causes eye, skin, and respiratory tract irritation. May be harmful if inhaled. Contact with eyes may cause severe irritation, and possible eye burns. May be absorbed through the skin. Causes irritation with burning pain, itching, and redness. Prolonged exposure may result in skin burns. Causes gastrointestinal irritation with nausea, vomiting and diarrhea. May cause kidney damage. May cause central nervous system depression, characterized by excitement, followed by headache, dizziness, drowsiness, and nausea. Advanced stages may cause collapse,

Brianna Galvan 13 July 2021 Experiment 1 Summer II 2021 unconsciousness, coma and possible death due to respiratory failure. May cause carboxyhemoglobinemia. Vapors may cause dizziness or suffocation. May cause blood changes. Overexposure may cause an increase in carboxyhemoglobin levels in the blood. Can produce delayed pulmonary edema. Because of its high volatility, airborne concentrations of methylene chloride can accumulate in poorly ventilated areas. Odor is a poor indicator of possibly dangerous air concentrations of methylene chloride. Possible cancer hazard based on tests with laboratory animals. Prolonged or repeated skin contact may cause dermatitis. May cause reproductive and fetal effects. Laboratory experiments have resulted in mutagenic effects. Chronic exposure may cause lung, liver, and pancreatic tumors. May cause conjunctivitis and/or corneal burns. Acetone C3H6O Molecular Weight: 58.08 g/mole Liquid pH (1% soln/water): 7 Boiling Point: 56.5 deg C Melting Point: -94 deg C Clear, colorless liquid. Extremely flammable liquid and vapor. Vapor may cause flash fire. Causes eye irritation. Breathing vapors may cause drowsiness and dizziness. Causes respiratory tract irritation. Aspiration hazard if swallowed. Can enter lungs and cause damage. Prolonged or repeated contact may dry the skin and cause irritation. Produces irritation, characterized by a burning sensation, redness, tearing, inflammation, and possible corneal injury. Vapors cause eye irritation. May be absorbed through the skin. Repeated or prolonged exposure may cause drying and cracking of the skin. May cause irritation of the digestive tract. May cause central nervous system depression, characterized by excitement, followed by headache, dizziness, drowsiness, and nausea. Advanced stages may cause collapse, unconsciousness, coma and possible death due to respiratory failure. Aspiration of material into the lungs may cause chemical pneumonitis, which may be fatal. Inhalation of high concentrations may cause central nervous system effects characterized by nausea, headache, dizziness, unconsciousness and coma. Causes respiratory tract irritation. May cause motor incoordination and speech abnormalities. Prolonged or repeated skin contact may cause dermatitis. Chronic inhalation may cause effects similar to those of acute inhalation. Matsushita et al. exposed human volunteers 6 hours/day for 6 days at 500 ppm acetone and found hematologic changes including significantly increased leukocyte and eosinophil counts and decreased neutrophil phagocytic activity. Pre-Lab Questions 1. Demonstrate the befits of a soxhel extractor instead of a simple extraction, for instance, in a round-bottom flask? Soxhlet extraction can extract multiple times Possible full spectrum of extraction Less amount of Labor (usage of hands) 2. Illustrate the mechanism regarding this ester hydrolysis. (Hint: use electron-pushing arrows).

Brianna Galvan 13 July 2021 Experiment 1 Summer II 2021

3. Since trimyristin is a triglyceride, specify what triglycerides signify? Triglycericles signify a type of compound, specifically a type of fat. Data: Weight=0.312g Rf=distance Spot moved/ distance solvent moved Melting point=53-54 Distance Spot moved=3.0cm % Yield=recovered/ theoretical *100= 0.72/2.467*100=29.19% Distance Solvent moved=6.1cm Rf=3.0/6.1=0.49 Observations Filtration is a funnel with a filter paper inside a ring iron ring clamp and then a beaker on the bottom to collect any of the liquid that falls through. The gravity filtration is added then the filter paper helped the solid from going straight down. Anything that is polar sticks to the silica, anything nonpolar moves with the mobile phase or the hexane ethyl acetate mixture. Brown color for the product in the beginning then when filter it will begin to be clear. Three Boiling chips were added to the clear solution and over in the fume hood. The product is a wax/ fat lipid. The acetone was added to dissolved crystallization which color was clear/yellowish. Conclusion: In this lab the melting factor of the crystals aid the isolation of trimyristin. The melting factor stages from 53-54. The two percent healing changed into low in comparison from the expected recovered 29.19%. the distance moved to forty-nine cm. The Ta extracted an impure product and resulted in a 30cm TLC confirmation solvent. Then later recrystallize the purifying trimyristin and purity resulting materials and data in experiment 2. Post Lab 4a.) Theoretical yield of myristic acid=moles*molar mass =0.0108*228.3709 =2.467 gm b.) Redeemed of myristic acid= 0.72g % yield=recovered mass/ theoretical yield *100 0.72/2.467*100 %yield =29.19% c.)  Rinse flasks and syringes used to transfer reactant and reagents  Use clean glassware  Calculate and weigh reagent amounts accurately 5.) What will occur to the melting point of your trimyristin result if your product remains wet when you record it?) Melting point of the solvent-contaminated trimyristin is lower than the purse compound. The most solvents being used in purification and has very low melting point during recrystallization depresses the melting point. 6.) In this experiment why didn’t we utilized ethanol to extract some trimyristin? This experiment would have reduced a step and could be recrystallized directly after filtration.

Brianna Galvan 13 July 2021 Experiment 1 Summer II 2021 The ethanol it will soluble in water so you cannot separate two layers, whereas if you use dichloride methane it will be in soluble in water so you can easily separate from the water. Reference:  Organic Chemistry II Laboratory – CHEM 3125 Lab Manual, Department of Chemistry Texas A&M University – Kingsville, Dr. Jason Abrams  YouTube, Tamuk Chemistry Department, 3 July 2020, www.youtube.com/watch? v=3IXkB-Tu1FY....