Part 2: Hydrolization
4) To the glycol add MeOH and H2SO4.
Runne - SWIM would true for epoxide. Yields seem higher. Also easier to distill. As long as you don't add too much buffer, the worst that will happen is that you will have some epoxide and some glycol (?).
5) Reflux for 3 hours.
Runne - You will see a color change about an hour into the reation. Usually yellow/orange juice color to a more brown/red tone.
6) After reflux, load contents into sep funnel and separate bottom (ketone) layer.
Runne - Once again, adding water seems to help extraction.
7) Extract ketone with DCM and pool extracts
Runne - ENSURE that the temperature of the reaction has lowered to well below 35C or so (DCM BP 39). BAD things happen when you add DCM to hot solution BAD BAD things.
Wash extracts with NaOH and separate in funnel (bottom layer has the goods).
Runne - SWIM usually thinks Bicarb is fine but SWIM is not an expert in this arena. ALSO - it seems to really clean up the solution if you mix/swirl the solution for a while (more than 5 minutes) then let settle.
9) Strip off DCM via distillation.
10) Recover ketone via vacuum distillation.
Runne- If you go unbuffered, you should note that ketone and epoxide have boiling points that are close together. You will see a change from a more yellow color to a slightly more green tinted more "see through" type of liquid which is ketone. OR, you may not. Bees seem to have different experiences with the actual color of the final ketone.
I do not consider myself an expert on the subject. Other comments/changes/corrections would be more than welcome.
Runne