01-20-04 17:42
No 483663
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?
(Hive Addict)
01-20-04 17:55
No 483666
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.
Patriotism is often an arbitrary veneration of real estate above principles - George Jean Nathan
(Newbee)
01-20-04 18:35
No 483676
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.
(Hive Addict)
01-20-04 18:46
No 483685
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.
Patriotism is often an arbitrary veneration of real estate above principles - George Jean Nathan
(Newbee)
01-20-04 18:51
No 483687
There is no DH20 wash in the benzo wacker, only bicarb, NaCl (skip this), and NaOH. Should a water wash be done last?
(Hive Addict)
01-20-04 18:59
No 483688
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.
Patriotism is often an arbitrary veneration of real estate above principles - George Jean Nathan
(Hive Addict)
01-21-04 05:40
No 483804
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.
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(Newbee)
01-21-04 10:46
No 483850
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.