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. This is FRIEDEL-CRAFTS ACYLATION AND COLUMN CHROMATOGRAPHY Not acid base extra

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Question

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This is  FRIEDEL-CRAFTS ACYLATION AND COLUMN CHROMATOGRAPHY Not acid base extraction. There will not be distillation. WE ONLY USE: FRIEDEL CRAFT ACYLATION, TLC, COLUMN CHROMTOGRAPHY AND NMR Analysis. Based on the above methods can anyone answer the following question?

During this lab you will perform an extraction. In your notebook, draw a flow chart that includes all the pertinent details for the extraction (solvents, products, amounts, impurities, drying agents, etc.) This is NOT a flow chart for the entire procedure, just a description of which compounds and solvents are in which layer at each part of the extraction.

Thank you

Explanation / Answer

1)Friedel crafts acylation reaction of aromatic substrate is carried out usng acetyl chloride as an acylating agent and the catalyst an unhydrous Lewis acid. using organic solvents like nitrobenzene or CS2 etc. Then pour into ice-water mixture with stirring.

1) Extract the mixture with solvents like pet. ether / ethyl acetate /chloroform/ DCM etc. & separate two layers.

2)If the mixture of the product is obtained tested on TLC , then go to column chromatography to separate products from impurity .If solid is obtained carry out crystallization using different solvents of varying polarity. Start with less polar solvent first ,like pet ether or n-hexane , then go to polar solvent like ethyl acetate or chloroform if necessary.

3) After separation remove the solvent under vacuum, to get the product. If product is liquid then distill under reduced pressure & if solid partial crystallization should be carried our.

4)Take m.p. /B.p.

5)Once you get pure compd. i.e. single spot on TLD then take NMR by dissolving in CDCl3 using TMS as a standard.

6)Take IR to detect C=O functional group.

7) Propose correct structure.