Bwiti (PVC-Analog Taste-Tester)
02-05-02 04:34
No 265292
      PdCl2 Costs Too Much ! !  Bookmark   

  If someone wanted to convert 500ml safrole into     MDP-2-P, using PdCl2, what's the least amount of PdCl2 that can be used? There's a synth in T.S.2, page 66, that uses 500g safrole/53g PdCl, but shit, that stuff costs alot. tongue

  Love my country. Fear my government.
 
 
 
 
    PrimoPyro
(Hive Prodigy)
02-05-02 04:51
No 265301
      Re: PdCl2 Costs Too Much ! !  Bookmark   

Have you even considered the tried and true performic route? I know this is not what you asked for, but I just wanted to bring it up. It is most certainly cheaper.

I do not know how much PdCl2 you would need.

                                                   PrimoPyro

Vivent Longtemps la Ruche!
 
 
 
 
    blaztoff
(Hive Bee)
02-05-02 11:36
No 265403
      Re: PdCl2 Costs Too Much ! !  Bookmark   

500ml safrole or grams safrole. Well close to equivalent wieght for these purposes anyway. But lets see. P-Benzo=2 grams PdCl2 per 150-170g sfrole. 02 wackers= 3g PdCl2 per 300grams safrole. Well Id say anywhere from 5-10gr PdCl2 for 500ml safrole. At current price 15.00g I say 85-150 dollars for PdCl2
 
 
 
 
    Rhodium
(Chief Bee)
02-05-02 12:21
No 265419
      Re: PdCl2 Costs Too Much ! !  Bookmark   

I would definitely reccommend isomerization (Vacuum/KOH) followed by a buffered performic oxidation. The yields may even be higher using that method.

Besides, the writeup in TSII uses way too much PdCl2 than necessary, there are more economic writeups at my page.
 
 
 
 
    Bwiti
(PVC-Analog Taste-Tester)
02-05-02 14:11
No 265452
      Re: PdCl2 Costs Too Much ! !  Bookmark   

"there are more economic writeups at my page."

  Right after this post, I'll head over to your site and do some serious fucking reading. I was really psyched about using palladium, but I'll save that for an allylbenzene(other than sweet safrole) that I can afford to fuck-up on. In my dreams, I haven't done a performic for a while..Is formic acid still safe to buy? The smell of acetic acid is more tolerable to me, but I haven't seen enough write-ups on a peracetic to feel comfortable using it. Thanks for the advise folks!cool

  Love my country. Fear my government.
 
 
 
 
    Rhodium
(Chief Bee)
02-05-02 14:41
No 265458
      Re: PdCl2 Costs Too Much ! !  Bookmark   

The peracetic sure works (and is well covered in the literature). Just follow Semtexiums writeup to the letter, andif it is still unclear, just ask him. Formic acid is not especially suspicious, it has loads of OTC uses. If you decide to go performic, use the method buffered by carbonate, it is really next-generation technique.
 
 
 
 
    cheeseboy
(Hive Bee)
02-05-02 19:52
No 265552
      Re: PdCl2 Costs Too Much ! !  Bookmark   

Using Cupric Chloride as a catalyst charger will enable you to use minimal Palladium. I think it's methyl man's benzo wacker on ../rhodium.  The CuCl keeps the Palladium chloride alive and kicking throughout the wacker oxidation run. just a suggestion, cheese hasn't tried it.

 Familiar with the Oxone route? Nice. OTC and CHEAP!

May The Source Bee With You....Always.

  - OB1KNoBee
 
 
 
 
    Vibrating_Lights
(Hive Bee)
02-05-02 20:37
No 265561
      Re: PdCl2 Costs Too Much ! !  Bookmark   

Go with oxone.. total cost of oxidation salt $2per Lb  Noj reports doing 450gms in a 5 gallon bucket with 1 lb of oxone,2gallons H20,2l MeOH.can't get any cheaper than that.
Vl_
 
 
 
 
    RoundBottom
(Hive Bee)
02-05-02 20:41
No 265562
      Re: PdCl2 Costs Too Much ! !  Bookmark   

are you concerned about maximizing yields or keeping costs low? 

in SWIMs experience, the benzo wacker produces greater returns on safrole than the ISO-peracid-hydrolosis route.  the main difference is that you can do all 500mL at once with a peracid, while you'd probably have to break up the benzo wacks into 2, as they aren't very scalable.

is SWIM way off base?  SWIM has been struggling to get more than 50% yield from (baal's) buffered performics... getting a lot of unreacted ISO mixed with the ketone (1/4 to 1/3 is ISO).  benzo wack yields were consistantly 75%-80%.

i learned a thing or two from charlie dontcha know.
 
 
 
 
    ChemicalSolution
(Hive Bee)
02-05-02 20:54
No 265570
      Re: PdCl2 Costs Too Much ! !  Bookmark   

Isn't the scale (from JOC article) 0.5mmol PdCl2/50mmole alkene?  This amounts to around 90g safrole/1g PdCl2.  Or is this too little PdCL2 for the common up-scaled reaction?

xoxo-Julia
 
 
 
 
    noj
(Hive Addict)
02-05-02 23:20
No 265623
      Re: PdCl2 Costs Too Much ! !  Bookmark   

VL, that was a mistake. It was 2Kg oxone. I divided instead of multiplying when making it into lbs. Sorry for the confusion. But still, that's $14 compared to $100.

Real men cook naked.
 
 
 
 
    potisgood
(Newbee)
02-27-02 22:32
No 274434
      Re: PdCl2 Costs Too Much ! !  Bookmark   

Look at my EtONO wacker.  It uses 4g PdCl2 per 500 g safrole.
 
 
 
 
    Sunlight
(Pioneer Researcher)
02-27-02 23:53
No 274480
      Re: PdCl2 Costs Too Much ! !  Bookmark   

What is your yield postisgood ? Succesful amination ? It is important becuase you can think like me you got a 70 %+, but amination showed ketone was not really pure, about a 85 % or so.
 
 
 
 
    foxy2
(Distinctive Doe)
02-27-02 23:56
No 274481
      Re: PdCl2 Costs Too Much ! !  Bookmark   

Palladium prices have droped a bunch lately, its now back at 1999 price levels.  I think the PdCl2 prices should follow soon.

http://www.engelhard.com/eibprices/DPCharts.aspx?MetalName=Palladium



Make a Difference Donate Now!! (http://www.lp.org/drugwar/)
 
 
 
 
    Moriarty
(Hive Bee)
02-28-02 07:27
No 274612
      Re: PdCl2 Costs Too Much ! !  Bookmark   

I know this isn't completely on topic, but I decided to include this thought after foxy2's comment on the price of Palladium.  It's not original, just a reminded.  Palladium is like $380 an oz.  It would take all of like $425 to make ~48 grams of the stuff.  That's like $9 a gram, which really beats the $20-$25 a gram someone who IS Moriarty has been paying for it.  Not to mention that, I believe, bullion is less suspicious to buy than PdCl2.  I wouldn't mention it at all, accept SWI Bwiti sounds like he's looking for a long term solution.

Who wants to play cops and dope fiends?
 
 
 
 
    noj
(Hive Addict)
02-28-02 07:44
No 274617
      Re: PdCl2 Costs Too Much ! !  Bookmark   

I used to think about using a Pd mesh screen attatched to a stirring unit in such a way that it would agitate through the solution. Don't know if that would even work, but it would make it easy to reuse the palladium.


Chaque un son gout
 
 
 
 
    Moriarty
(Hive Bee)
02-28-02 07:56
No 274620
      Re: PdCl2 Costs Too Much ! !  Bookmark   

I don't think elemental Palladium won't work.  If I understand the concept, Pd salts are the only thing that will work, most of which aren't real effective.  I think its Palladium Acetate and Palladium Chloride that'll work with any real success and I don't know much about the acetate.  Would be nice if it did.

Who wants to play cops and dope fiends?
 
 
 
 
    Bwiti
(PVC-Analog Taste-Tester)
02-28-02 08:47
No 274635
      Re: PdCl2 Costs Too Much ! !  Bookmark   

"SWIM has been struggling to get more than 50% yield from (baal's) buffered performics..."

  Ouch! Oh well, at least you can re-process the isosafrole. In my dreams, I'd like to let the iso react with a buffered peracetic for 48 hours in an attempt to get higher yields, because I'm worried that too much iso mixed with the MDP2P will fuck-up the formation of the bisulfite.

"accept SWI Bwiti sounds like he's looking for a long term solution."

  At first, I was looking for a long term solution, but over time that has been replaced by desperation.tongue

  Thanks for all your help folks! Where else can you get this much help, and not have to pay a fee.cool

  Love my country. Fear my government.
http://www.gothicradio.com
 
 
 
 
    potisgood
(Newbee)
02-28-02 21:20
No 274872
      Re: PdCl2 Costs Too Much ! !  Bookmark   

My yield from 180 g safrole was 140 g distillate.  I have figured, though, that I loose most of my yield during distillation.  Before I distilled, I had 170 g of rather pure looking oil in the flask (wine red color, but transparent, as opposed to black and gooey).  When I fractionally distilled the 140 g of distillate to purify it, I lost 5% to the distillation.  Also, the distillate I collected is really fucked up.  Instead of one peak corresponding to ketone, I got two.  One was around 120C and the other around 150C.  Neither was safrole.  I even took drip rate vs. temperature data and plotted a graph.  The graph showed that there were two peaks in the collection as well.  My theory is that both of these peaks are relatively pure ketone, but one of them (probably the higher one) is an azeotrope that the ketone forms with either its polymer or some unhydrolyzed acetal.  I suspect this, because I have found that the acetal forms a minimum azeotrope with safrole, even in very small quantities.  The lower fraction was pale flourescent green (like lemon-lime powerade) and the higher fraction was more like piss yellow.  Both fractions were about equal in size.  I have yet to aminate it, as I am trying out a new procedure for then amination and need to perfect it first.  I would post the graph I made, but I don't know how.
 
 
 
 
    pickler
(Greenhorn)
02-28-02 22:26
No 274918
      Re: PdCl2 Costs Too Much ! !  Bookmark   

Swim got some pdcl2 for $500. 50 grams of it. Buy it in bulk, it's the way to go.

We'll soon FIND OUT if I'm a chemist or not!
 
 
 
 
    Aurelius
(Hive Bee)
03-02-02 08:50
No 275659
      Re: PdCl2 Costs Too Much ! !  Bookmark   

forget bulk, just ask a friend (ehh, bwiti? you want PdCl2?  talk baby, talk.)
 
 
 
 
    cheeseboy
(cheese head)
03-02-02 10:25
No 275700
      Re: PdCl2 Costs Too Much ! !  Bookmark   

If PdCl can be re used then it's a good idea, can it? kinda like RP used over and over again. except cheese always loses close to a third of the catalyst in each run.... noj : How are your yiels with the oxone epoxidation/thermal rearrangement?

Cheeseboy-a whiteboy with Soul Like a black guy without soul
May The Source Bee With You Always.
 
 
 
 
    noj
(Hive Addict)
03-02-02 20:10
No 275813
      Re: PdCl2 Costs Too Much ! !  Bookmark   

50-60% to ketone. I haven't done the thermal.


Chaque un son gout
 
 
 
 
    Bwiti
(PVC-Analog Taste-Tester)
03-03-02 19:18
No 276293
      Re: PdCl2 Costs Too Much ! !  Bookmark   

"forget bulk, just ask a friend (ehh, bwiti? you want PdCl2?  talk baby, talk.)"

  Yes, that would be great! I'm a chemical-whore.tongue

"I would post the graph I made, but I don't know how."

  It would be cool if The Hive allowed you to post your own pics, rather than links to images. Don't let that stop you. Scan your graph, make it as small as possible, then save it as a gif. Go to the chemistry section of poppies.org and post your gif there, then link it to this thread. Peace! cool

  Love my country. Fear my government.
http://www.gothicradio.com