Author Topic: Dr Drool method Viable?  (Read 2303 times)

myhero

  • Pupae
  • **
  • Posts: 80
Re: Dr Drool method Viable?
« Reply #120 on: June 02, 2013, 01:52:46 PM »
You ll be fine. You re doing good!

Flight

  • Larvae
  • *
  • Posts: 23
Re: Dr Drool method Viable?
« Reply #121 on: June 03, 2013, 05:14:51 PM »
Vacuum was connected to begin distilling the ketone and the water pump for the recirculating aspirator was dead.  The same day the LCD screen on my computer died. When it rains it pours.  A replacement 3/4hp water pump was installed, the old one was 1/2hp.  That little bit of extra power made a huge difference it the amount of vacuum it pulled through the aspirator. 

A vigreux column was installed, vacuum started and heat was turned on.  Between about 152 and 160 a beautiful Mt. Dew like color came through the condenser.  Total yield from 150 Iso was 210g Glycol and finally ~90g MdP2P.  There were a bunch of mistakes made, simply pouring stuff from one bottle to another several times definitely lowers yields.  A few drops were lost here and there and that adds up.

The Methyl Man Reductive Amination with AL/HG will hopefully be performed today or tomorow. 

What are people using to get the gas into the solution.  I can't seem to find any glass tubing, except on ebay.  Something in the 5mm OD would be good, then it would fit into the thermometer adapter.  Is polyethylene tubing good enough to use for the HCL gas?  This could probably be found at a hardware store. 

Any thought or advice are always appreciated.
THanks,
Flight   

Similar to what Pbint said, there was a lot of remaining liquid in the original flask, nothing polymerized.  Is this just waste product or should another distillation be attempted to see if any more ketone comes over? 
« Last Edit: June 05, 2013, 02:29:07 AM by Flight »

syn

  • Larvae
  • *
  • Posts: 12
Re: Dr Drool method Viable?
« Reply #122 on: June 03, 2013, 08:02:07 PM »
It's called a gas dispersion tube, they sell them on ebay.

Flight

  • Larvae
  • *
  • Posts: 23
Re: Dr Drool method Viable?
« Reply #123 on: June 03, 2013, 08:33:52 PM »
@Syn,

 I was trying to find more of a local solution.  In Argox's gassing write up he has polyethylene pictured.  It seems this would be a low cost and convenient gassing tube.  Eventually Ill get a real one from ebay.

Anyway look at this:
menda.descoindustries.com/PDF/ChemicalResistanceChart.pdf

Sneak

  • Junglist
  • Subordinate Wasp
  • ***
  • Posts: 105
Re: Dr Drool method Viable?
« Reply #124 on: June 04, 2013, 01:16:40 AM »
Yeah I'm sure iv seen written in more than one place you can use the tubing mentioned for HCl gassing, Flight. Just have a look at the ghetto gasser solutions for more info.

This might help..
http://www.erowid.org/archive/rhodium/chemistry/hcl-gas.html
« Last Edit: June 04, 2013, 01:20:59 AM by Sneak »
If you really want to enjoy a pure, clean product the only way... is to make it yourself...

You miss 100% of the shots you don't take...

Flight

  • Larvae
  • *
  • Posts: 23
Re: Dr Drool method Viable?
« Reply #125 on: June 06, 2013, 08:47:46 AM »
MM's AL/Hg amalgamation began, instructions followed out by reading Methyl Man's write up and Gonzo's pictorial.  Everything seems to be running well.  All colors matching the pictorial.  A 3in stir bar was obtained and placed in with 27.5g coffee ground Aluminum foil and MeOH.  The ketone was placed in the addition funnel along with nitrometh and more MeOH.  Everything proceed just as the write up described, exothermic heating and MeOH dripping like a fountain through the condenser.

The one issue is that the solution at the bottom of the flask is very thick.  The stir bar was having serious issues stirring.  A bunch a MeOH was added and the problem still persists.  There are no signs of shiny aluminum flakes and it looks like it was a success.  Eventually the flask was unclamped and shaken repeatedly then placed back in the clamp and stirring commenced.  This will be allowed to go through the evening and tomorrow the final stages and gassing will be performed.

Hopefully positive results will be posted.

Thanks,
Flight


Flight

  • Larvae
  • *
  • Posts: 23
Re: Dr Drool method Viable?
« Reply #126 on: June 06, 2013, 07:54:43 PM »
The flask was emptied into another container and the NaOH will be poured in and mixed.  It is a very thick sludge and quite a bit a MeOH was added just to remove the contents from the original flask. 

Has this been the case for everyone else performing MM's amalgam?  Not sure the 3in stir bar will be able to move any of the solution it's so thick.  An overhead stirrer could be rigged up using an electric screwdriver, but the only kind of whisk usable would be metal (Either the type to whisk eggs or the type for making cookie batter).

Any thoughts or ideas are always appreciated,
Thanks,
Flight
« Last Edit: June 06, 2013, 08:41:58 PM by Flight »

zgoat65

  • Subordinate Wasp
  • ***
  • Posts: 103
Re: Dr Drool method Viable?
« Reply #127 on: June 09, 2013, 04:16:06 AM »
This thread at WD may bee useful to you

hxxp://www.wdrestored.com/forums/viewtopic.php?f=38&t=1448&hilit=ptfe+stirrers
If you build a man a fire, he'll be warm for a day.
If you set a man on fire, he'll be warm for the rest of his life

Flight

  • Larvae
  • *
  • Posts: 23
Re: Dr Drool method Viable?
« Reply #128 on: June 10, 2013, 07:00:53 PM »
The MM amalgam was performed the other day and gassed last night. The toluene was very clean it was washed with, 1x 500ml sodium bicarb, 1x 500ml dH2O, 1x 500ml brine and finally 500ml dH2O.  The toluene was poured into a jar containing 32.5g anhydrous MgSO4, stirred occasionally and placed into another completely dry jar after an hour.

The H2SO4 was dripped over HCL dampened NaCl and the tube placed inside the jar of toluene/product.  Immediately clouds started to form and fall to the bottom.  Gassing was stopped and the jar was placed in the freezer.  It was only suppose to be in there for 30-45 minutes, but stayed in longer because someone fell asleep.  The product was filtered out and dried and there was only ~3g of product.

Gassing was attempted again, but there was no more precipitate.  The toluene turned from a clear water color to a yellow color.  MgSO4 was placed into the jar in an attempt to draw out some more water and then it will be gassed again.

Why was there so little product that crashed out?  From 25g ketone shouldn't there be more then 3-4 grams?

Any ideas or advice would be appreciated,
Thanks,
Flight
« Last Edit: June 10, 2013, 07:03:29 PM by Flight »

Sneak

  • Junglist
  • Subordinate Wasp
  • ***
  • Posts: 105
Re: Dr Drool method Viable?
« Reply #129 on: June 10, 2013, 08:56:40 PM »
How long did you gas for?
If you really want to enjoy a pure, clean product the only way... is to make it yourself...

You miss 100% of the shots you don't take...

Flight

  • Larvae
  • *
  • Posts: 23
Re: Dr Drool method Viable?
« Reply #130 on: June 10, 2013, 09:03:51 PM »
the first gassing ran for only a few minutes maybe 3-10 total, but there was precipitate almost immediately.  The gassing bubbles would slow down and more H2SO4 released.  The Toluene turned a slight yellow color.  the next gassing was done several hours later, probably for the same amount of time maybe 3-10 minutes. 

A 125ml addition funnel was filled with H2SO4 and dripped onto the HCL dampened NaCl.  Once the 125ml of H2SO4 ran out the gassing stopped.

Perhaps the gassing isn't being done for long enough?  How long should it take to gas and get out all the goodies?  This is really annoying.

Thank you so much for the reply,
Flight
« Last Edit: June 10, 2013, 09:07:32 PM by Flight »

Sneak

  • Junglist
  • Subordinate Wasp
  • ***
  • Posts: 105
Re: Dr Drool method Viable?
« Reply #131 on: June 10, 2013, 09:48:30 PM »
Could you solvent have become wet from being in freezer so long. Perhaps your further drying will help.
If you really want to enjoy a pure, clean product the only way... is to make it yourself...

You miss 100% of the shots you don't take...

Flight

  • Larvae
  • *
  • Posts: 23
Re: Dr Drool method Viable?
« Reply #132 on: June 10, 2013, 10:08:22 PM »
Quote
Could you solvent have become wet from being in freezer so long. Perhaps your further drying will help.

I was kind of thinking the same thing, I'm hoping so.  Is the yellow color change normal after gassing?  I'll keep you posted.

Thanks,
Flight

ImAMANGUYS

  • Pupae
  • **
  • Posts: 84
Re: Dr Drool method Viable?
« Reply #133 on: June 11, 2013, 03:35:33 AM »
From experience and what it sounds like the amalgam may have not run to completion? The only amalgams i've not gotten great yields on were because of poor stirring. Usually a redish or pink nonpolar solvent i've heard indicates that it is wet, but if the nonpolar goes yellow IME its close to done or gotten a bit wet. Try drying and gassing again if you're worried!

Sneak

  • Junglist
  • Subordinate Wasp
  • ***
  • Posts: 105
Re: Dr Drool method Viable?
« Reply #134 on: June 11, 2013, 07:41:10 AM »
I was going to say the yellow may be the HCl if you have gassed alot already.

The thing to remember is I haven't done these reactions. Although iv done a lot of reading. You should take note of what the more experienced bees have to say over my comments. I like to try have some input though. :)
If you really want to enjoy a pure, clean product the only way... is to make it yourself...

You miss 100% of the shots you don't take...

myhero

  • Pupae
  • **
  • Posts: 80
Re: Dr Drool method Viable?
« Reply #135 on: June 11, 2013, 07:57:16 AM »
as a last resource add some water and extract your toluene with water HCl with a titration. So you'll know if water in NP was the issue or just bad yields in your red. oxidation..

fishinabottle

  • Subordinate Wasp
  • ***
  • Posts: 129
Re: Dr Drool method Viable?
« Reply #136 on: June 11, 2013, 01:38:06 PM »
Stop gassing. Just put it in the fridge and and wait.

Overnight.

You can boil away some ot the nonpolar to remove azeotropically water present but thats not a must.

I suppose you have a good amount of unreacted ketone and other questionable shit in your extract. This prevents instant crystallisation. It prevents complete crystallisation too but thats a minor problem, most will come. Not as much as you hope though.

From my experience time is the key. Fucking further around with it completely ruined it not only once for me, resulting not in bad but in zero yields.

/ORG

Flight

  • Larvae
  • *
  • Posts: 23
Re: Dr Drool method Viable?
« Reply #137 on: June 11, 2013, 06:06:25 PM »
After adding MgSO4 and shaking the hell out of it, I gassed it again.  Thankfully another bumper crop fell to the bottom.  After filtering I filled the jar with more MgSO4 and have been letting it sit overnight, shaking and stirring periodically.  All of the yellow tint is gone and toluene/product looks as it should (clear).  About to gas again and hopefully there is another happy result. 

What is the best way to stir through the sludge of the amalgam?  A 3 inch and 1 inch stir bar are the only available options.  Are there any tricks to learn about?  Planning to run another of MM's Al/Hg amalgam today, but want to be sure it runs to completion and there is no unreacted ketone.  So 20+ gram yields from 25 grams of ketone can be realized.

As always, thanks for all the assistance,
Flight
   
« Last Edit: June 11, 2013, 07:09:19 PM by Flight »