How to work-up reaction using separatory funnel?

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>> Monday, June 18, 2012

separatory funnel, liquid-liquid extraction
As you know, to get a pure compound is not an easy task. Here, I am going to write about the work-up process (liquid-liquid extraction) using separatory funnel, one of the methods for the purification of crude compound. I hope it will be helpful for you. In this method, two immiscible solvents, aqueous and organic solvent (ethyl acetate, methylene chloride etc) are used which allows the removal of water soluble impurities present in the reaction mixture. 

Work-up procedure

Transfer the reaction mixture completely into the separatory funnel using the appropriate organic solvent. "Be cautious to close the stopcock". After that pour distilled water into the separatory funnel. Hold the stopper tightly and shake the reaction mixture gently. "Be sure to release the pressure- hold the stopper tightly, invert the funnel pointing outlet upwards and open the stopcock (See the video below)".
I want to share my bitter experience here. Once, while doing work-up (during shaking), I forgot to release the pressure. As soon as I kept the separatory funnel to stand, solvent splashed out of the separatory funnel through the stopper. Oh gosh! You can imagine the situation.:(

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