Author Topic: 1 Mole Oxone Scale Up  (Read 4057 times)

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Vibrating_Lights

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1 Mole Oxone Scale Up
« on: June 06, 2002, 08:41:00 PM »
Swim found this at the park

1 mole  of alkene is charged into a 3 gallon bucket along with 1.3L of EtOH. Then 3750 Ml of DH2O is added and stirring commenced with a 3"stirbar.  Then there was added 727gms of Oxone.  Ph of the solution checked to be 2-3.  Imediatly there after starts the addition of 225 gms of Sodium bicarbonate. At the end of the addition the Ph Was 7.4(Phenol red indicator).  This is stirred for 5 hrs during which time the temp will climb to 37.c peaking at around 1.45 hrs. And the PH is 5.6 at the end of the rxn 

The author here must have been low on dcm and did this.
It would be bettr to use alot of dcm  but.....

The contents of the bucket were allowed to settle then 300gms of sodiumbicarbonate was added very quickly to cause a mass release of co2 at the bottombubbling all of the epoxide to the surface.  when bubbling slowed to where the epoxide was visable the epoxide was decanted off with some of the  aquious layer There was probably a good portion of epoxide left in there.  He let setle again  and this time poured off the aquious layer into another bucket leaving the crystals.He extrracted  the crystals with a bit of EtOH and added it to the aquious layer.  Then he added the 200ml of dcm that he had to the aquious layer and stirred for 5 mins.  He seperated the dcm layer and added it to the epoxide that the ppoured off originaly.  then he seperated the dcm/epoxide layer and washed it 4x with saturated bicarb. 
The Dcm was distilled off in a 2l after which 1500ml of 15%H2So4 was added.
 The hotplate was set to 90.c  This maintained a temp of 80.c in the 2l.  this was refluxed for 3.5 hrs.  the mix was cooled afterwards with D-ice and a little more water was added to get the ketone to the bottom..
The top layer Was poured into the 150ml of dcm and shaken.  this was seperated and the dcm was added to the ketone..
This was washed withsaturated bicarb x2 and 5%NaOh  x1.

The crude ketone was placed into a 500ml rbf and distilled.

140ml of DCM Atm 39.c
Under conventional vaccume distillation(gaduge was)fucked
150-153 89 Ml of Piss yellow PMP2P
16 gms of tar was further extracted with MeOH from the distillation flask afterwards.