Storing MDP2P in DCM?

[Mercury]

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?

[abolt]

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.

[Mercury]

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.

[abolt]

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.

[Mercury]

There is no DH20 wash in the benzo wacker, only bicarb, NaCl (skip this), and NaOH. Should a water wash be done last?

[abolt]

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.

[GC_MS]

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.

[Glasya]

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.