- Work-up
In
chemistry , work-up refers to the series of manipulations required to isolate and purify the product(s) of achemical reaction .Typically, these manipulations include:
* quenching a reaction to deactivate any unreacted reagents
* cooling the reaction mixture or adding an "antisolvent" to induce precipitation, and collecting or removing the solids byfiltration ,decantation , orcentrifugation
* removal of solvents by evaporation
* separating the reaction mixture into organic and aqueous layers byliquid-liquid extraction
* purification bychromatography ,distillation orrecrystallization For example, in the
Grignard reaction betweenphenylmagnesium bromide andcarbon dioxide in the form ofdry ice gives the conjugate base ofbenzoic acid . The desired product, benzoic acid, is obtained by the following work-up: [cite book | title = Introduction to Organic Laboratory Techniques: A Small Scale Approach | author = Donald L. Pavia | year = 2004 | publisher = Thomson Brooks/Cole | isbn = 0534408338 | pages = 312-314]# The reaction mixture containing the Grignard reagent is allowed to warm to room temperature in a water bath to allow excess dry ice to evaporate
# Any remaining Grignard reagent is quenched by the addition of water
# Dilutehydrochloric acid is added to the reaction mixture to protonate the benzoate salts, as well as to dissolve the magnesium salts. White solids of impure benzoic acid are obtained.
# The benzoic acid is decanted to remove the aqueous solution of impurities, more water is added, and the mixture is brought to a boil with more water added to give a homogenous solution.
# The solution is allowed to cool slowly to room temperature, then in an ice bath to recrystallize benzoic acid.
# The recrystallized benzoic acid crystals are collected on aBuchner funnel and are allowed to air-dry to give pure benzoic acid.ee also
*
Flow chemistry References
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