I need a purification flow chart for this Organic Chemistry experiment: Reaction
ID: 570907 • Letter: I
Question
I need a purification flow chart for this Organic Chemistry experiment:
Reaction steps:
1.To a tared 100-mL round-bottom flask add 0.5 mL of -caprolactone and determine the mass added.
2. Add a stir bar, 50 mL of absolute ethanol, and 0.2 mL of concentrated sulfuric acid.
3.Place a water-cooled reflux condenser on top of the round-bottom flask.
4.Mount the flask in your sand bath on a magnetic stirrer and heat the sand to reflux the solution for 30 minutes.
5. Remove the reaction from the sand bath and allow it to cool for 10 minutes.
6. Add 800 mg of sodium bicarbonate to the reaction flask and stir. Keep stirring until gas evolution subsides. (Note this will take several minutes.)
7. Vacuum filter the solution through a small Hirsch funnel. Transfer the solution to a 100 mL beaker with a boiling chip.
8. Boil the solution down under a stream of air until about 1-2 mL of solution remains. (Note: solids may be present at this point.)
9. Remove the beaker from the sand bath and cool to room temperature.
10. Add 7 mL of methyl t-butyl ether (MTBE) and 7 mL of water to the solution and transfer it to a large test tube.
11. Mix well, allow layers to settle, and separate the layers with a Pasteur pipet. Put the organic layer aside.
12. Extract the aqueous layer two more times with 7 mL portions of MTBE.
13. Next, extract the combined organic layers once with saturated sodium chloride.
14. Dry the organic layer with anhydrous sodium sulfate.
15. Pre-weigh a 50 mL beaker and boiling stone. Boil off the solvent on a sand bath with compressed air. The product will be an oily liquid.
16.Weigh your product. Set aside about half of the product in a vial for later GC-MS and FT-IR and comparison to a standard. Use the rest (0.5-1 mL) for Stage 2.
Step 1. Trans-esterification of s-Caprolactone OH Excess Q H2S04 Catalytic Ethyl 6-HydroxyhexanoateExplanation / Answer
Flowchart for the experiment:
1) weigh an 100 ml round bottom flask=Wf
2) Take 0.5ml e-caprolactone in the flask and weigh it again =weight of flask +e-caprolactone=w,Thus weight of e-caprolactone=w-Wf
3) Add 50 ml ethanol+0.2 ml conc sulfuric acid to it and reflux the mixture in a sand bath with magnetic stirrer for 30 minutes
4) Remove from the bath and cool the reaction mixture
5) Add 800 mg sodium bicarbonate, and keep stirring until all the evolving gas escapes
vacuum filter and transfer to a 100 ml beaker
6) Add boiling chips and boil the rxn mixture until its volume reduces to 1-2ml only
7) Extraction of compound from the rxn mixture:
cool and add 7 mL methyl t-butyl ether (MTBE) +7 ml water
Mix well and seprate the layers (organic and aqueous ) using Pasteur pipet
Using 7 ml MTBE,repeat the steps 7 ,two more times to extract more of the compound from the aqueous layer
8) combine all the organic liquid from step 7
9) Add saturated saturated sodium chloride,and extract organic layer once more
10)Add anhydrous sodium sulfate to absorb even traces of water if present
11) take a weighed 50 ml beaker ,add boiling stone and boil off the organic liquid on a sand bath with compressed air,pure product will be left over as oily liquid
12)weigh the product,and separate parts for GC-MS and FT-IR analysis
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