Homework Help Question & Answers

PROCEDURE CAUTION!!! Nitric acid and sulfuric acid are strong and corrosive acids. For that reason, avoid...

PROCEDURE CAUTION!!! Nitric acid and sulfuric acid are strong and corrosive acids. For that reason, avoid inhaling its vapors

of the nitrating mixture. After completing the transfer of the entire contents of the MN test tube to test tube A, remove

B. COMPLETE LOS ESPACIOS EN BLANCO 1. DATA TABLE OF THE REACTION (8) OCH, OCH + HNO3 + H2804 NO2 Molecular formula Quantity [

2. TABLE OF EXPERIMENTAL RESULTS (33) Theoretical yield for the product (3) g Weight of crude product (3) g Yield of crude pr

PROCEDURE CAUTION!!! Nitric acid and sulfuric acid are strong and corrosive acids. For that reason, avoid inhaling its vapors or causing any contact with the skin or clothing. Wear your protective glasses at all times. Use the extractors to work with these acids. A. Nitration of methyl benzoate 1. Preparation of the reactants. In the extractor you will find a burette with concentrated sulfuric acid, a second burette with concentrated nitric acid, clearly identified. Familiarize yourself with the scales of both burettes to be able to measure the volume of the acids correctly. Then, transfer to a large, clean, dry test tube labeled "A" 1.0 mL of concentrated sulfuric acid (H2SO4), introduce the thermometer (do not remove it from the test tube until the end of the experiment) and cool its contents to 0 °C, placing the test tube with a 3-fingered clamp in an ice/water bath. Add from the third burette 0.50 mL of methyl benzoate to test tube "A" that is at temperature of 0 °C. Then, remove the test tube from the ice/water bath and let the temperature of the test tube reach about 20 °C, slightly shaking the contents of the tube with the thermometer. Re-cool the test tube until its contents again indicate the temperature of 0 °C. While cooling the test tube "A", prepare another test tube (medium or small size), clean and dry, labeled "MN" (nitrating mixture). In the extractor, carefully transfer to the "MN" test tube first 0.4 mL of concentrated nitric acid (HNO3) and then 0.4 mL of concentrated sulfuric acid. Shake the warm mixture carefully with a clean, dry glass rod. 2. Nitration With a clean, dry Pasteur-type dropper, transfer slowly (this is the crucial part of the experiment and dropwise the nitrating mixture from the "MN" test tube to the test tube "A" containing the acidified methyl benzoate found in the ice/water bath , but in such a way that the temperature stays between 10 and 15 ° C. If the reaction temperature is lower, the reaction is very slow and if it is higher than 15 °C, a greater amount of secondary products could be formed, which can be controlled by maintaining the temperature in the indicated range by means of a slow addition
of the nitrating mixture. After completing the transfer of the entire contents of the "MN" test tube to test tube "A", remove the water /ice bath and let the temperature of the reaction mixture in tube "A" reach about 20 °C, stirring occasionally for 40 minutes, period of time in which the reaction will have come to an end. 3. Isolation of the raw or crude product Prepare a water / ice bath in the metal container. Add some crushed ice (+0.3 mL, unmeasured) in a clean beaker of 25-100 mL. Before the ice has melted, pour the reaction mixture from the "A" tube at once onto the ice in the beaker, which in turn is inside a water/ice bath. Without shaking the contents of the beaker, allow the mixture to stand until the formation of the crystals of the methyl m-nitrobenzoate has come to an end. Filter the crude product by suction in the microscale funnel, followed by about 2-3 mL of cold distilled water to complete the transfer of the product to the funnel. Rinse the reaction tube with 2 mL of cold water and add them to the suction funnel. Add another 2 mL of cold distilled water to complete the washing of any acid residue and continue the suction until the product is almost dry. Place the solid on a weighing paper, minimize the amount of water pressing it with a filter paper until it shows no moisture. Then weigh the solid, determine the % of the crude and place 1 mm of the solid in the capillary for melting point. 4. Purification of methyl m-nitrobenzoate by recrystallization To recrystallize, transfer the crystals of the crude product to a clean and dry 10 mL Erlenmeyer flask. With a dropper, transfer dropwise as much ethanol as necessary to cover the crude methyl m-nitrobenzoate, - 1 mL. With the transformer in 15 units of scale or sand band between 40 and 55 °C, heat the contents of the Erlenmeyer by stirring on the sand bath until the ethanol is hot or close to boiling. Observe if all the crystals have dissolved. If they have not dissolved, add another bit of ethanol (3-5 drops) and boil again until the crystals are completely dissolved. Then, cover the Erlenmeyer, let it reach room temperature (5 minutes), then cover, place it in a water/ice bath (5 minutes), until the crystallization of the methyl m-nitrobenzoate is quantitative. Filter the recrystallized product by suction using about 2 mL of cold ethanol (0-5°C) to complete the transfer of the product to the microscale suction funnel. Suction until the product stops dripping, place the solid on weighing paper or watch glass, wait 3 minutes to ensure it does not contain ethanol. 5. Determination of weight and melting point Weigh the recrystallized and dry product, transfer it to a small, clean and labeled test tube. Determine the melting point of both the crude and recrystallized methyl m-nitrobenzoate. The melting point of pure methyl m- nitrobenzoate is 78 ° C. Complete the following table with your experimental data and show the labeled test tube containing the product to your teacher.
B. COMPLETE LOS ESPACIOS EN BLANCO 1. DATA TABLE OF THE REACTION (8) OCH, OCH + HNO3 + H2804 NO2 Molecular formula Quantity [g] moles C. Ho Og | HNO3 H₂SO4 C&HAND, Molecular mass [g/mol] CA 136.1 63.01 18.079 149.15 0.544 0.409 1.83 10.86 3.97X103958X103 1.8x102 2.0 x109 10.5 im 1.51910m 1.83g1m3 1.20 BP-83c/up-10°C Volume [ml] Density (g/mL] 1.094 Physical constant [°C]
2. TABLE OF EXPERIMENTAL RESULTS (33) Theoretical yield for the product (3) g Weight of crude product (3) g Yield of crude product (4) % Product purification technique (2) Solvent used to purify the product (2) Weight of pure product (4) g Percentage yield of pure product (4) % % to °C Melting point range of the crude product. (3) Melting point range of the pure product, obtained by you (3) Melting point range of the pure product, obtained by your partner (3) Reference melting point (2) to °C °C
0 0
Add a comment
Answer #1

Sign Up to Unlock the answer FREE

Already have an account? Log in

& Fins According to the data given by you: Molecular (C&H ₂ O 2 HNO₂ 63.01% 98.079 149,15 loomua 136.15 . Quontity (g) 0.54 1givenas. :- OCH 20 HNO, would be the line 149. 15 of m-nitro- The reaction which takes place a OCH, +HNO3 + H₂SO4 → From the09 oo - We use the process of recrystallization for purification of methyl m-nitrobenzoate 10 which is extracted out itself a

Add a comment
Know the answer?
Add Answer to:
PROCEDURE CAUTION!!! Nitric acid and sulfuric acid are strong and corrosive acids. For that reason, avoid...
Your Answer:

Post as a guest

Your Name:

What's your source?

Earn Coin

Coins can be redeemed for fabulous gifts.

Not the answer you're looking for? Ask your own homework help question. Our experts will answer your question WITHIN MINUTES for Free.
Similar Homework Help Questions
  • QUESTION: Write a flow scheme for the work-up. THE WORK UP:

    QUESTION: Write a flow scheme for the work-up. THE WORK UP: C. Work-up (save all layers) and Isolation of Product MgBrCl Benzoic acid Transfer the mixture into a test tube. Rinse the beaker with about 3 mL of regular (not anhydrous) diethyl ether and pour the washings into the test tube. There should be two distinct layers in the test tube Remove the aqueous layer (to be discarded) and shake the ether layer with about 2 mL of 3 M...

  • For the nitration of methyl benzoate: a. Which product did you get? What evidence do you...

    For the nitration of methyl benzoate: a. Which product did you get? What evidence do you have for this? b. Was your product pure? What evidence do you have for this? Explain your evidence. c. Draw the mechanism for the product you got. For the bromination of acetanilide: a. Which product did you get? What evidence do you have for this? b. Was your product pure? What evidence do you have for this? Explain your evidence. c. Draw the mechanism...

  • Place 3.0 g of salicylic acid in a 125-ml Erlenmeyer flask. Carefully add, stirring constantly, 6...

    Place 3.0 g of salicylic acid in a 125-ml Erlenmeyer flask. Carefully add, stirring constantly, 6 mL of acetic anhydride, followed by 10 drops of concentrated sulfuric acid. Swirl the contents of the flask so that the reactants are thoroughly mixed. Stopper the flask with a one- hole cork fitted with an inverted Pasteur pipet to prevent condensation of water in the reaction flask during heating on the steam bath. Heat the flask in a boiling-water or steam bath for...

  • this is the procedure of melting point experiment ( preparation acetanilid) I want the summarize of...

    this is the procedure of melting point experiment ( preparation acetanilid) I want the summarize of this procedure EXPERIMENTAL PROCEDURE Measure 0.100 to 0.125 g of aniline (in dropper bottles near the balances) into a tared reaction tube from the microscale kit and record the weight to the nearest milligram. Add 2 mL of distilled water and 6 to 7 drops (an excess amount, 21 drops =1 mL) of acetic anhydride. Stir the mixture for about 4 minutes untiha solid...

  • Running the Reaction Add 0.100 g benzil and 0.30 mL 95% ethanol to a 3-mL conical vial. Place a s...

    Determine the theoretical yield and limiting reagent Running the Reaction Add 0.100 g benzil and 0.30 mL 95% ethanol to a 3-mL conical vial. Place a spin vane in the vial and attach an air condenser. Heat the mixture with an aluminum block (90-100°C) while stirring until the benzil has dissolved (see inset in Tech- nique 6, Figure 6.1A). Using a 9-inch Pasteur pipette, add dropwise 0.25 mL of an aqueous potassium hydroxide solution' downward through the condenser into the...

  • 3-5 pls Post-Laboratory Questions-EXP 3 Nitration of Aromatic Compounds Name: Due after completing the lab. 1....

    3-5 pls Post-Laboratory Questions-EXP 3 Nitration of Aromatic Compounds Name: Due after completing the lab. 1. Why is concentrated sulfuric acid employed in this reaction? What is the electrophile that is produced by the reaction of sulfuric acid and nitric acid? 2. Why is it important to maintain the reaction temperature low and the addition of nitric acid-sulfuric acid mixture carried out slowly? 3. Explain why concentrated H2SO, not concentrated HCl, was used in this experiment? 4. Which ring of...

  • numbers 1-3 Post-Laboratory Questions-EXP 3 Nitration of Aromatic Compounds Name: Due after completing the lab. 1....

    numbers 1-3 Post-Laboratory Questions-EXP 3 Nitration of Aromatic Compounds Name: Due after completing the lab. 1. Why is concentrated sulfuric acid emploved in thie on? What is the electrophile that is produced by the reaction of sulfuric acid and nitric acid? 2. Why is it important to maintain the reaction temperature low and the addition of nitric acid-sulfuric acid mixture carried out slowly? 3. Explain why concentrated H2SO4, not concentrated HC1, was used in this experiment? 4. Which ring of...

  • Write out your separation scheme for this experiment. 1. Heat 75 mL of water to 90...

    Write out your separation scheme for this experiment. 1. Heat 75 mL of water to 90 °C in a 250-mL beaker. 2. While the water is being heated, place 250 mg of salicylic acid, 1 drop of 85% phosphoric acid and 0.5 mL of acetic anhydride in a test tube. Add a boiling chip to the mixture and gently shake it in order to mix the reactants. 3. Heat the tube in the beaker of water at 85 - 90...

  • PROCEDURE 1. Place a reaction tube into a 5-mL Erienmeyer and tare. Add between 0.275- 0.300g...

    PROCEDURE 1. Place a reaction tube into a 5-mL Erienmeyer and tare. Add between 0.275- 0.300g of salicylic acid. Record on the data sheet. 2. Transfer the reaction tube and 5-ml Erienmeyer to the hood. Add a boiling chip, 2 drops of 85% phosphoric acid, and about 0.70 mL of acetic anhydride to the reaction tube. Mix well. 3. Place a 50-ml beaker containing about 20-mls of water on a hot plate or in the sand bath. Allow the water...

  • QUESTIONS 1. What is the purpose of the sulfuric acid (yes, it's a catalyst, but why...

    QUESTIONS 1. What is the purpose of the sulfuric acid (yes, it's a catalyst, but why is it a catalyst? What is it doing that makes the reaction possible? Would the reaction just go slower without it, or would the reaction not go at all? Why?) 2. If isobutyl alcohol (2 methyl propanol) is used instead of tert butyl alcohol, a mixture of products is obtained. One the products is the same as the product obtained with the tert butyl...

ADVERTISEMENT
Free Homework Help App
Download From Google Play
Scan Your Homework
to Get Instant Free Answers
Need Online Homework Help?
Ask a Question
Get Answers For Free
Most questions answered within 3 hours.
ADVERTISEMENT
Active Questions
ADVERTISEMENT