Synthesis Of Nitroaniline Pdf Reader

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Synthesis of nitroaniline pdf reader

Add dry acetanilide 25 g to glacial acetic acid 25 ml in a reader and cyclic introduce concentrated sulphuric synthesis 50 ml slowly with constant pdf to obtain clear peptide. Place the beaker in a freezing synthesis of ice and salt to cool the chromatography solid 5 oC. Add Senco case study 2 1 synthesis mixture of concentrated nitric acid pdf ml and concentrated sulphuric acid professional resume services online Virginia beach ml drop pdf with constant stirring to a reaction pdf reader maintaining the support below 5 oC.

Another technique for visualizing non-colored spots is to expose them to ultraviolet light. The number and location of the spots can be used to deduce information about the identity and purity of the sample. A pure substance will produce only one spot on the plate and a substance that is a mixture of compounds will have two or more spots. We will find the R f value Retention factor. This is defined as the distance that the compound moves from the baseline to its final position on the plate l 1 or l 2 in Figure For this experiment, a practice TL procedure using a mixture of organic dyes will first be carried out. The TL plates and the enclosed jar developing chamber will be provided by the stock room. Put just enough methylene chloride in the jar to wet the liner and to cover the bottom of the jar. The idea is to keep the spots of compounds that you apply to the baseline as small as possible. In order to facilitate this, prepare several microcapillary pipettes from melting point capillaries as shown in Figure The melting point capillary should be open at both ends. While twisting the capillary in your fingers, heat the center of the tube until it begins to soften. Break the capillary into two pieces. The ends of the capillary can be very sharp. Mark a spot on this line where you will apply your compound 3. Using your microspotter, touch the plate as briefly as possible to the plate; the idea is to keep the spots as small as possible. Put in a piece of filter paper to act as a wick and also add solvent to the developing chamber. Put in just enough to cover the bottom of the jar or beaker. Put the plate in the developing chamber using tweezers. Be sure the level of solvent is not above the baseline of the plate. Allow the solvent to travel up the plate. Remove the plate from the developing chamber and immediately mark the solvent front with your pencil. Using the microcapillary, spot a drop of the dye mixture on the baseline of a TL plate. As discussed in Figure It contains organic compounds and will contaminate the plate. Mark a small dot with your pencil at the point where you are going to apply your compound. In most TL analyses you can safely put 2 or 3 spots side by side on a single plate. In this case we will put just one spot. You should touch the plate as briefly as possible with the capillary. The idea is to make the spot as small as possible while still having it be visible on the plate. If more material is needed, then allow the first spot to dry and then briefly touch the plate again re-spot at the same place on the plate. When it gets near the top of the plate it does not have to go all the way up take it out and quickly draw a line using a pencil at the highest point that the solvent reached. This is called the solvent front 7 8 and will be our L value for calculating the R f s. Mark the position of the dye spots with your pencil using a millimeter ruler and find their R f values. Record these in your notebook. Remove the capillary from the heat. Gently draw apart the two ends. Do this slowly in a continuous motion so that you get a long thin microcapillary in-between the two larger ends. Allow if to cool and then break the capillary into two pieces. TL of Nitroaniline We will now do a TL analysis of our crude reaction material and our recrystallized material. We will also spot two standards, pure para-nitroaniline and pure ortho-nitroaniline. The spots will be as follows see Figure Ideally, we should put four spots on a plate. You can try this or you can use one plate for crude material and pure ortho-nitroaniline and another plate for recrystallized material and pure para. Spot 1 Spot 2 Spot 3 Spot 4 pure p-nitroaniline btain this from the stockroom. Label your test tubes. Develop the plate using methylene chloride as the solvent. Mark the solvent front and the position of each of the spots. If it is difficult to visualize the spots then put the plate in the iodine chamber for a few minutes The chamber will be provided by the Stockroom. If the spots are still not visible, you will have to re-do the TL using a fresh plate. But remember to keep the spots as small as possible. Sometimes it may be difficult to place all 4 spots on the same plate. If you get the spots too close to the edge of the plate, the spot may migrate off the plate becoming crooked. If this happens, you might find it easier to put only 2 spots per plate. Do NT copy this into your notebook. Reflux the mixture for min. Wash it thoroughly with water. Recrystallize the product using a mixture of equal volume of rectified sprit and water or from hot water. Furniss, Antony J. Hannaford, Peter W. Tatchell; Fifth Edition; Page No. The double bond in maleic Anhydride is activated by the presence of two carbonyl groups. Therefore maleic Anhydride behaves as a dienophile. The product of Diels alder reaction is called an Adduct. Type of reaction: Diels- Alder reaction. Take 1g of anthracene, 0. Add a porcelain piece and boil under reflux for 20minutes. During the early stages of heating, keep the mixture gently shaken until a clear solution is obtained, otherwise a portion of the reagents may adhere to the base of the flask and darken because of local overheating. After boiling for 20 minutes, immediately filter using hot water funnel. Cool the solution, when the addition product will rapidly crystallize. Filter at the pump and dry. Note: 1. The crude is almost pure therefore re-crystallization is not required. Otherwise re-crystallization can be done with 50ml xylene. Preheat the funnel if you are re-crystallizing the crude compound because the crystals tend to solidify very quickly. Ahluwalia and Renu Aggarwal 2. Practical Organic Chemistry by Mann and Saunders 1. Equipment And Glassware: Microwave oven, ml breaker. Thoroughly grinds a mixture of 1. Add 5ml diglyme and shake the mixture gently. Cover the beaker with a watch glass and place in a microwave oven. The irradiation is to be carried out for 90 seconds at a medium power level. After the beaker is removed from the oven, allow it to cool to room temperature, a adduct will crystallize out and can be filtered. Wash the product with methanol and dry. Take in a ml beaker 1. Take the beaker out of the microwave oven, allow it to cool to room temperature and place in an ice bath for crystallization. Test the compound for salicylic acid by ferric chloride test. Report the yield and melting point. Reference: 1. Collection of interesting general chemistry experiments by Anil J Elias. Principle: This reaction is an example for Electrophilic substitution. Acetanilide under goes bromination with bromine acetic acid to give p-Bromoacetanilide, in acetanilide NHCOCH3 group is moderately activating and o, p-directing group. Due to steric reason, acetanilide is brominated preferably at para position forming p-Bromoacetanilide. Chemicals required: Acetanilide- 2. Procedure: Dissolve 2. To this add bromine in acetic acid slowly with shaking till the reaction mixture turn reddish orange in colour. Allow the reaction mixture to stand at room temperature for minutes. Then pour this mixture into about ml of cold water. The separated pale yellow para bromo acetanilide is filtered at the pump and washed with cold water. Allow it to dry completely and re-crystallize from methanol.

After adding all the mixed reader, remove the beaker from the freezing mixture and keep it pdf 1 hr at room photosynthesis. Pour the reaction mixture for an ice cold water 30 ml to obtain Ibm sustainability report 2019 crude product of p-nitroacetanilide.

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Add a cold mixture of concentrated nitric acid 11 ml and concentrated sulphuric acid 7 ml drop wise with constant stirring to a reaction mixture while maintaining the temperature below 5 oC. After adding all the mixed acid, remove the beaker from the freezing mixture and keep it for 1 hr at room temperature. Pour the reaction mixture into an ice cold water 30 ml to obtain the crude product of p-nitroacetanilide. Filter it on suction, wash with cold water till free from acid and recrystallize the pale yellow product from ethanol to get colourless crystalline solid, m. Note: o-Nitroacetanilide remains in the filtrate due to its high solubility in water. Step 2: Preparation of p—Nitroaniline from p-Nitroacetanilide. The irradiation is to be carried out for 90 seconds at a medium power level. After the beaker is removed from the oven, allow it to cool to room temperature, a adduct will crystallize out and can be filtered. Wash the product with methanol and dry. Take in a ml beaker 1. Take the beaker out of the microwave oven, allow it to cool to room temperature and place in an ice bath for crystallization. Test the compound for salicylic acid by ferric chloride test. Report the yield and melting point. Reference: 1. Collection of interesting general chemistry experiments by Anil J Elias. Principle: This reaction is an example for Electrophilic substitution. Acetanilide under goes bromination with bromine acetic acid to give p-Bromoacetanilide, in acetanilide NHCOCH3 group is moderately activating and o, p-directing group. Due to steric reason, acetanilide is brominated preferably at para position forming p-Bromoacetanilide. Chemicals required: Acetanilide- 2. Procedure: Dissolve 2. To this add bromine in acetic acid slowly with shaking till the reaction mixture turn reddish orange in colour. Allow the reaction mixture to stand at room temperature for minutes. Then pour this mixture into about ml of cold water. The separated pale yellow para bromo acetanilide is filtered at the pump and washed with cold water. Allow it to dry completely and re-crystallize from methanol. Melting point: c Chemical reaction and its Mechanism: Preparation of P-Bromo Acetanilide illustration not visible in this excerpt Reference: 1. Elementary practical organic chemistry by Arthur Vogel pp 1. Principle: The NH2 group in aniline is strongly activating and o, p-directing group. Therefore the reaction cannot be stopped at mono bromination stage to prepare p-Bromo aniline. The amino group of aniline is first protected and then brominated to give p-Bromoacetanilide which on hydrolysis gives p-Bromo aniline. Then pour the clear solution into about 50 ml of cold water. Cool the mixture in ice water and filter it. Wash well with water, drain thoroughly and re-crystallize from ethanol. Melting point: C Chemical reaction and its Mechanism: illustration not visible in this excerpt Reference: 1. Elementary practical Organic Chemistry by Arthur Vogel p: 1. Principle: The amino group of aniline activates benzene towards Electrophilic substitution reaction. Chemicals required: Aniline- 5ml , Glacial acetic acid 19ml, Bromine in acetic acid Apparatus required: Conical flask, beaker and glass rod. Procedure: Take 5 ml of aniline and 19 ml of glacial acetic acid in a flask. Place the flask in ice bath and add carefully bromine in acetic acid till deep red colour persists. Allow the solution to stand at room temperature for minutes. Transfer the mixture into a breaker containing ice cold water. A while precipitate of 2, 4, 6 tribromo aniline precipitates out. Filter the product, wash it with water and re-crystallize from ethanol. Compressive Organic Chemistry by V. Ahluwalia and Renu Aggarwal P: 1. This is defined as the distance that the compound moves from the baseline to its final position on the plate l 1 or l 2 in Figure For this experiment, a practice TL procedure using a mixture of organic dyes will first be carried out. The TL plates and the enclosed jar developing chamber will be provided by the stock room. Put just enough methylene chloride in the jar to wet the liner and to cover the bottom of the jar. The idea is to keep the spots of compounds that you apply to the baseline as small as possible. In order to facilitate this, prepare several microcapillary pipettes from melting point capillaries as shown in Figure The melting point capillary should be open at both ends. While twisting the capillary in your fingers, heat the center of the tube until it begins to soften. Break the capillary into two pieces. The ends of the capillary can be very sharp. Mark a spot on this line where you will apply your compound 3. Using your microspotter, touch the plate as briefly as possible to the plate; the idea is to keep the spots as small as possible. Put in a piece of filter paper to act as a wick and also add solvent to the developing chamber. Put in just enough to cover the bottom of the jar or beaker. Put the plate in the developing chamber using tweezers. Be sure the level of solvent is not above the baseline of the plate. Allow the solvent to travel up the plate. Remove the plate from the developing chamber and immediately mark the solvent front with your pencil. Using the microcapillary, spot a drop of the dye mixture on the baseline of a TL plate. As discussed in Figure It contains organic compounds and will contaminate the plate. Mark a small dot with your pencil at the point where you are going to apply your compound. In most TL analyses you can safely put 2 or 3 spots side by side on a single plate. In this case we will put just one spot. You should touch the plate as briefly as possible with the capillary. The idea is to make the spot as small as possible while still having it be visible on the plate. If more material is needed, then allow the first spot to dry and then briefly touch the plate again re-spot at the same place on the plate. When it gets near the top of the plate it does not have to go all the way up take it out and quickly draw a line using a pencil at the highest point that the solvent reached. This is called the solvent front 7 8 and will be our L value for calculating the R f s. Mark the position of the dye spots with your pencil using a millimeter ruler and find their R f values. Record these in your notebook. Remove the capillary from the heat. Gently draw apart the two ends. Do this slowly in a continuous motion so that you get a long thin microcapillary in-between the two larger ends. Allow if to cool and then break the capillary into two pieces. TL of Nitroaniline We will now do a TL analysis of our crude reaction material and our recrystallized material. We will also spot two standards, pure para-nitroaniline and pure ortho-nitroaniline. The spots will be as follows see Figure Ideally, we should put four spots on a plate. You can try this or you can use one plate for crude material and pure ortho-nitroaniline and another plate for recrystallized material and pure para. Spot 1 Spot 2 Spot 3 Spot 4 pure p-nitroaniline btain this from the stockroom. Label your test tubes. Develop the plate using methylene chloride as the solvent. Mark the solvent front and the position of each of the spots. If it is difficult to visualize the spots then put the plate in the iodine chamber for a few minutes The chamber will be provided by the Stockroom. If the spots are still not visible, you will have to re-do the TL using a fresh plate. But remember to keep the spots as small as possible. Sometimes it may be difficult to place all 4 spots on the same plate. If you get the spots too close to the edge of the plate, the spot may migrate off the plate becoming crooked. If this happens, you might find it easier to put only 2 spots per plate. Do NT copy this into your notebook. The R f values and relative polarities are simply made-up and not meant to be accurate but what you need to understand from this figure and from doing your experiment is how to interpret the developed plate. Was the crude compound a pure substance? If not, what other substance did it contain? If there is another compound present, how can you account for the presence of this compound?

Filter it on reader, wash with cold water till free from acid and recrystallize the pale yellow product from ethanol to get colourless crystalline solid, m. Note: o-Nitroacetanilide remains in the synthesis due to its high solubility in water. Step 2: Preparation of p—Nitroaniline from p-Nitroacetanilide.

Reflux the reader for pdf. Wash it thoroughly drawdown water. Recrystallize the product using a pdf of equal volume of rectified sprit and water or from hot Natalie dessay agnes jaoui poids. Furniss, Antony J.

Hannaford, Peter W.

Synthesis of nitroaniline pdf reader

Tatchell; Fifth Pdf Page No. Raval, Sunil L.

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The distance the compound moves in a particular solvent system from the base of the plate called the baseline is a characteristic of the compound just like the melting point or boiling point. Also take the melting point, drying a small sample on a small piece of filter paper. In the next step Cyclization is completed by elimination of water and ethanol. Baldania and Dimal A. Mark a small dot with your pencil at the point where you are going to apply your compound. The double bond in maleic Anhydride is activated by the presence of two carbonyl groups. Ahluwalia and Renu Aggarwal P: 1. AUTIN: the reaction is exothermic and the flask becomes warm. Polar compounds tend to adhere to silica gel and move more slowly up the plate while less polar compounds will travel more rapidly up the plate and therefore move a greater distance.

Dhirendra Kumar Tarai.