If one cannot distill MDP2P from the DCM after all the appropriate washes, would it ok to store it in the freezer while in the DCM?
Are you telling me that you cannot distill something with a B.P. of 40 Celcius.
AFAIK, raw ketone should be distilled A.S.A.P.
Distillation is not the problem, time is the problem. Can it be stored in the freezer? I don't see it causing a problem considering that MM recommends to store the raw ketone immediately after the wacker if one were to stop at that point.
IME, If the Ketone has been distilled it will store in the freezer without DCM.
If it hasn't then it should store for a short amount of time but I would distill A.S.A.P.
Make sure you do bicarb/DH2O/Brine washes prior to storage.
There is no DH20 wash in the benzo wacker, only bicarb, NaCl (skip this), and NaOH. Should a water wash be done last?
Apologies, never seen a benzo wacker.
Swim has stored impure ketone in the freezer after neutralising the acid without too many problems.
If you have a mixture of DCM and raw ketone do the following: Wash order is 2 x Bicarb, 2 x DH2O, 1 x Brine.
Store in cool and distill A.S.A.P.
Try to supply more detailed info when you want help.
Do not store DCM in the Refridgerator/Freezer in a metal container. On a particularly hot day SWIM tried to cool down a drum of DCM in the refridgerator, in order to keep fuming to a minimum prior to opening, only to find that the drum had virtually imploded. :P
In the old days, chemists sometimes traded (and stored) benzaldehydes as their bisulfite. I guess these compounds aren't as prone to O2-oxidation as the free benzaldehyde, but I'm not sure.
SWIM washed 2x with Bicarb and 2x with NaCl followed with 3x NaOH and never had a problem. I have seen a lot of complaints with washing with NaCl – lot of emulsions and the sort, but letting it sit for 20 min and then with a little swirl everything settled out and it was really easy to separate.
SWIM ran 2 reaction at the same time once and got called away, after 8 hour reflux with no time SWIM put glass stoppers in all 3 necks of the 2 2L flasks and put them both in the freezer for 2 days at -20. Everything after that worked fine but this was before the DCM was added or washes were done.