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Apparatus for Simple Distillation

Apparatus for Simple Distillation. Organic Reaction. Adding starting material Work- up Extracting Washing Drying Purification Recrystallization Distillation Chromatography. Organic Reaction Work- Up. Extracting Washing Drying. Organic Reaction Work-Up Extraction.

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Apparatus for Simple Distillation

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  1. Apparatus for Simple Distillation

  2. Organic Reaction • Adding starting material • Work- up • Extracting • Washing • Drying • Purification • Recrystallization • Distillation • Chromatography

  3. Organic Reaction Work- Up • Extracting • Washing • Drying

  4. Organic Reaction Work-UpExtraction Liquid-liquid extraction is based on the principle that if a substance is soluble to some extent in two immiscible liquids, it can be transferred from one liquid to the other by shaking the two liquids together Pulling the desired compound out of a mixture Organic Layer Neutral Organic (Usually) Aqueous Layer Charged Molecule Inorganic Salts

  5. Organic Reaction Work-UpExtraction You have 1g desired compound and other impurities in your reaction bottle 0.9g your desired compound in organic layer 0.1g your desired compound in aqueous layer

  6. Organic Reaction Work-UpExtraction Pouring the aqueous layer back to separatory funnel and adding organic solvent Organic layer Containing desired compound 0.1x0.9=0.09g Aqueous layer Containing desired compound 0.1x0.1=0.01g

  7. Organic Reaction Work-UpExtraction Combine two organic layer 0.9+0.09=0.99g desired compound recovered in organic layer

  8. Organic Reaction Work-UpExtraction Pouring the water layer back again to separatory funnel Organic layer Containing 0.01x0.9=0.009g desired compound Aqueous layer Containing 0.01x0.1=0.001g desired compound

  9. Organic Reaction Work-UpExtraction Combine three organic layer 0.9+0.09+0.009=0.999g desired compound recovered in organic layer

  10. Organic Reaction Work-UpWashing • Wash Pulling unwanted impurities away from the desired compound • Use what you know about the impurities to decide on • appropriate aqueous washes • Washes should only be 10-50% of the volume of the • solution • Repeat each wash 2 or 3 times

  11. Organic Reaction Work-UpWashing Organic layer Aqueous layer NaHCO3

  12. Organic Reaction Work-UpWashing Organic layer Aqueous layer HCl

  13. Organic Reaction Work-UpDrying Magnesium sulfate -------good general drying agent, suitable for nearly all organic liquids Brine------saturated NaCl

  14. Organic Reaction Purification • Recrystallization • Distillation • Chromatography

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