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Lab: ISOLATION OF A NATURAL PRODUCT BY STEAM DISTILLATION

Procedure

Weigh approximately 5.0 g of spice into a 250 mL round bottom flask and add 150 mL of water. Assemble a simple distillation apparatus.
Careful heating is important or frothing may be a problem.

Distill about 50 mL of liquid into a 150 mL Erlenmeyer flask (or beaker). The distillate may be cloudy.

Add the distillate to a separatory funnel followed by 10 mL of dichloromethane. Gently shake to achieve good agitation and separate the lower layer (CH2Cl2 layer). Repeat the extraction again using a second 10 mL portion of dichloromethane.

Combine the dichloromethane extracts, add enough anhydrous magnesium or sodium sulfate to the dichloromethane and swirl until the liquid is no longer cloudy and there is no aqueous layer on top.

Decant the product into a tarred 50 mL beaker and evaporate all the dichloromethane by warming the beaker on a hot plate.

Ask your instructor on how to dispose of the remaining spice mixture.

Identify the structure of your natural product on the basis of its infrared spectrum.

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