Author Topic: DMF/O2 wacker miserable failure  (Read 1942 times)

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pooky

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DMF/O2 wacker miserable failure
« on: September 06, 2003, 03:31:00 AM »
P had some extra chems laying around,so P thought it fun to try DMF/O2 wacker.According to info on R's site and Hive, P tried 4 (75g safrole)at the same time,in the 2 l SRV.Increased the catalyst/Cu variably;3 with hardcore shaking and one with minor shaking every 15 minutes.Not a single one heated up on it's own(some say hot,some say cool),so P heated one up in a hot water bath,and O2 uptake was basically the same as the others.O2 drop in pressure in all of them was 70 to 75 psi over 10 hours,and not one produced ketone after the proper workup.I wonder where Grouch went right????

LaBTop

  • Guest
I know where you went wrong,
« Reply #1 on: September 06, 2003, 12:43:00 PM »
he used a stirbar, at max possible stirring of a very strong stirrer. He even mentioned the dent the stirbar made in the bottom of the carboy. LT/


Grouch

  • Guest
Here I am!
« Reply #2 on: April 18, 2004, 04:14:00 AM »
The dent in the bottom was due to the pressure inside the carboy.  The carboy was trying to become a sphere!


P had some extra chems laying around,so P thought it fun to try DMF/O2 wacker.According to info on R's site and Hive, P tried 4 (75g safrole)at the same time,in the 2 l SRV.Increased the catalyst/Cu variably;3 with hardcore shaking and one with minor shaking every 15 minutes.Not a single one heated up on it's own(some say hot,some say cool),so P heated one up in a hot water bath,and O2 uptake was basically the same as the others.O2 drop in pressure in all of them was 70 to 75 psi over 10 hours,and not one produced ketone after the proper workup.I wonder where Grouch went right????




You're being vague as hell!  According to what info at the Hive and Rhodium's site?  SRV?  Changing the amounts of catalysts?  Minor shaking?  No wonder nothing worked.  You should give exact details of your procedure or troubleshooting is very difficult.


pooky

  • Guest
Grouch!
« Reply #3 on: April 21, 2004, 06:10:00 AM »
Nice to have a response  after 6 months;hope your time off was well earned.
Well, all that was just an experiment one day...please notice that only one had minor shaking,the other 3 were abused horribly.As well, the catalyst was increased just to see what would happen..had the stuff sitting around,and was just fooling around.Discoveries are not made by following the same routine.
And SRV?Well P did not want to run a monster like you did,so used the old 2l pop bottle trick.Have since happily and successfully moved onto benzo wackers. ;)