Previous Chapter - 3.7 Analysis of crude product (WORKUP)

 

4. PURIFICATION


4.1 General approach

Step by Step: Time-sensitive

  1. Consult the literature. If conditions for successful purification of the compound have been reported, (Crystallization, Distillation, or Chromatography), follow the protocol.
  2. If literature is unhelpful, you must choose a purification method for your compound by following the Rules of Thumb:

For all other situations, use Column Chromatography.

  1. Save a small sample of the crude product mixture in a vial.
  2. Carry out the purification (for specific details, see Crystallization, Distillation, or Chromatography.) Keep everything.
  3. Collect major product components in tared flasks, and assign names to each component.
  4. Compare the components (usually by TLC) with the crude sample in the vial, and with the crude NMR, if any, to ensure that you have isolated the compounds of interest.
  5. Calculate the yield of each component, if the identity of the compounds is known.

Tips:

 

Next - 4.2 Column Chromatography