--------------------------------------------------------------------------

MDP2P production using the Spiceboy SRV/KRV
                                       
Posted on the Hive by Spiceboy 7/01/98

Question: Why is everyone afraid of pressure reactions? 'Cause they're 
dangerous, right? Well, somewhat, yes, No more so than many other things, tho.

After having listened closely to Osmiums tales of power about his pressure 
dreams, I meditated on the problem and came up with a WHOLE NEW APPROACH to an 
old problem. I didnt want to use a champagne bottle because of a few different 
reasons, most of them having to do with it being glass. Plus you cant see color 
changes thru a green bottle. Well get ready everyone for a new dawn... 
Introducing the SRV (Spice Reactor Vessel) a 'ketone generator, if you will, 
its so simple that you'll scream....

What you need: one 2 L coke bottle. One valve stem for a car tire. I found it 
easily... fits in the neck tightly... what you have to do is squeeze the base 
and deform the rubber to a slight oblong shape. You will be able to pull the 
stem up and cork the bottle with it from the inside out, if you will. This is 
your pressure vessel. It is very easy to wire the stem in using the nice wide 
collar that runs around the top of the bottle. Try to visualize. I have 
tested the apparatus to 2.5 atm successfully. At about 40lbs the fuckin thing 
BLEW THE VALVE STEM OUT of the bottle like a .60 cal. shell. I never did find 
it. Oh well, they're only a buck. Thats why I mention wire. Anyway this is the 
setup for the dream that is my next post, on the novel page, entitled LET THERE 
BE KETONE...


Part 2: Let there be ketone
---------------------------

I want to thank Osmium for the original inspiration.

This process will allow the reacting of one hundred grams of olefin w/ 2g of 
PdCl2, and 8g of CuCl2. There will be no oxygen tank. The reference the main 
part of this is based on indicate that air will serve as an able reoxidant, 
and it will.

The SRV is pressurized with a tire pump. (37-40 psi)

Dissolve 8 g CuCl2 in 80 ml MeOH.
Dissolve 2 g PDCl2 in 40-50 ml MeOH.
Mix 100 ml safrole w/ 200 ml MeOH.

* Pour it all in and add methanol to make 500 ml.
* Swirl and shake to mix.
* Pressurize to 40 psi.
* Shake like hell for 15-20 mins, repeat this hourly or more.

ORIGINAL REACTION RAN 21 HRS W/ 6-8 HRS STANDING TIME IN THE COOL.
So, actually, it ran about 14 hrs, w/ about 7 hrs standing.

Dont heat this stuff in any way while preparing. Heat favors aldehydes.
The refs say that isomerization is decreased with control over 2 factors:

1) you must keep the oxygen available.
2) you must keep it cool. Not cold, just cool...say around 20°C or so.

Contents are already acid, usually, but I like to hit it w/ some dilute acid 
before extraction.

This method is pretty close to OTC, and represents much testing and research. 
Not everyone had immediate results with it, but it is a very viable method.

--------------------------------------------------------------------------
Posted on the Hive by Spiceboy 11/18/98


This is an update on the SRV concept, including a detailed run w/ the unit.
In this dream the ratios were as:

        1 g PdCl2
        6 g CuCl2
        250 ml denatured alcohol
        50 ml ultra clean, vac distilled safrole

After mixing the copper salt w/ alcohol, it was chucked in the SRV.

Same for the PdCl2. Its probably better to put the palladium directly in
the SRV via funnel, than to put it in a separate beaker and trying to do
the mixing beforehand. The reason why is that the shit sticks to the beaker
and is hard to recover when transferring containers.

When you get it all in there, assemble the unit and THROW IN A STIRBAR
before you plug it up with the valve stem...this is a minor improvement
that makes a BIG difference, because it enables you to get a much more
turbulent agitation of the mixture...and that increases the oxygen uptake
dramatically.

This was done next;

Plug the unit. Pressurize it w/ the pump.

I have found that you cannot run the electric tire pumps off of a small
battery charger because it doesn't have the amps. Go out to your car and
pressurize on the ground beside it. Or take a car battery and set up a work
station at a bench, whatever.

Pressurize it for ten seconds. Shake it. Presurrize more. Shake it.
Pressurize it until it rock hard, all the while shaking strongly. You can
get a really good swirling-shaking action going on with the stir bar inside
of the unit. If you think about it, this is the principle that engineers
use to package spray paints in such a way that the contents can be readily
mixed, while being under pressure. I really cant emphasize enough the
difference this made in my dream. Your shaking effort is actually reduced,
while your mixing efficiency is exponentially increased. Shake some more.

I shook the unit vigorously, nonstop for two hours. Well, stopped every
ten minutes to relieve gases, and purge. Squeeze it while holding the valve
open,and purge two or three times. Away from your face. Have cold water
nearby to immerse the unit in intermittently, while repressurizing.
This improves uptake. Shake it. Shake it. See?

When you first place everything in the unit, the stuff is a light,
green-brown-golden. It evolves to gold-brown, then brown, then brick-red
at the end. Really hard shaking was used, and never let up on.

At the end, when it was brick red, I noticed a fine suspension of Pd
particles. Then, would purge and add new air. The particles would go away
for a short time and come back, so this was done a few times, and ,
evidently, as the reaction finished, the catalyst QUIT GOING BACK INTO
SOLUTION and would deposit as a fine, granular silt on the sides of the SRV
as you slowly rotate it.

The character of the solution seemed to change right about the time the
shit went from brown to dark red, too. It seemed less viscous, and kinda
acted like it was more easily agitated. I dont know how objective Im being
here, just thiught I'd add that.

Remember, Shake It Real Hard. There were vertical cracks appearing in the
unit at the end of the Rx, indicating that it was a hearty shaking affair,
replete with purge and binge...

Make up dilute acid. Others have said that it's not needed, but in my
dreams a much more efficient separation is achieved with dilute HCl being
used to bust everything up. Hit the stuff with about 200-300 ml of this.
It gets cloudy and tan-crap-greenish color and a HEAVY RED OIL falls out to
the bottom. But its full of catalyst. Get the buchner funnel and your
patience together. Assemble them. Filter all this crap about 3-4 times with
the paper I have, don't know about you. A clear red oil is obtained, and
believe it or not, ZERO TAR. ZERO.

The result? 37 ml of ketone from 50 ml safrole. Thats over 70%. Its
repeatable. It IS NOT A FLUKE. There was extremely little iso and even less
unconverted olefin. Removing the catalyst is a bitch, but its not really
bad. You do need vaccuum. It seems like denatured ethanol is superior, in
my dreams, to methanol as a substrate.

Well, there you have it. If anyone is not afraid of shaking for two hours,
this is a very viable way to get the stuff.....

Low temps seem to favor a better all-round set of kinetics for this reaction.

--------------------------------------------------------------------------
Posted on the Hive by Spiceboy 11/18/98
                                    
Addendum:

After about 45 minutes of prssure/ shaking, 2ml of water was added to the
mixture. This detail was added because it *may* have been important to
anyone else finding themselves in this dream. It maybe wasn't necessary,
but I have no way of knowing if/how much water is in the denatured (slx)
alcohol. The dihydrate was used, salt-wise.

--------------------------------------------------------------------------
Posted on the Hive by Spiceboy 11/27/98 

Well the final distilled product from these wacker/SRV's is a light, clear 
yellow-green. It comes over @170-175°C. It smells weird, too... post-purity 
yield is 55%-60%....some messy technique. also, it glows a real cool green 
under black light,too...

The ONE REAL criteria in these reactions is the O2: Pd, IMHO. With more Pd, 
your results improve. With air, use less Pd. But air makes it easy for anyone. 

--------------------------------------------------------------------------
Posted on the Hive by Spiceboy 98/12/07

This is a major finding in the sequence of SRV-type reactions.

I have found that in the using of Pd powered Wacker oxidations that there
is a 'window' of Pd amount used that greatly influences factors such as
pressure and shaking, and generally makes the air Wacker a little hard to
predict.

I will tell you this;

Using 1 g Pd to 50 g alkene WILL produce MDP2P, but ONLY if you put out
your MAX effort when it comes to shaking, and you make a TOP effort to keep
the purge/binge thingy rollin'...(lotta air.A L O T )

If you do not perform with great vigor, you may not achieve conversion. I
was confused when my new found reaction only returned the safrole to me one
night, and I began wondering why...then I remembered that BIG HUMONGOUS
SKUNK joint that I smoked, and that, due to it, I really didn't get the
full focus of my att'n span goin' on, so, was a little lax in the
re-airing, and a little lax in the power of my shaking.

But the colors I posted werent right this time. They werent changing
definitively. After the processing I got my oil back.

I dreamed this dream again, and re-duped my original conditions, with
earth-quake shaking, GONZO repressurizations, and attention to all details.

*POW!*

(ketone appears)

not the chemist, the chemical....

So, this means that I am onto something. But I am telling you that this is
probably the most physically demanding method you could ever dream up, ...

I started wondering,...hmmm...How about if you could get the results with
your half-ass performance, and not have to feel like you've been at the
deltoid machine at Golds Gym...

This took me back to JOC 34.

and this ratio...

3 g PdCl2
18 g CuCl2

(I used 65 g of alkene, double distilled.)

I went the 'wimpy' process, which was still fairly robust shaking, and ,
maybe, 75% of the attention to the re-airing process.

Guess What!?!?

KETONE. Yes there was one BITCH of an emulsion, but good lord, thats a
lotta metal salt. It all cleaned up w/ a few passes thru the ol'
Buchner....

Yield: After the processing, where I estimate I lost 10%, I got back 32 g
of very light yellow oil that smells nothing like safrole. It has a
heavier, softer smell, with an element of something spicy.

so the moral of this story is:

Use more Pd and get results that are more consistent.

Again, it WILL work with less, but you will work your ass off...and I am
not sure, but I think I repressurized it (dont have my notes) 32 times.
This was calculated by the volume of the bottle, the amt. of O2 req'd, and
the amt. of O2 in air(~21%)...

If you use 3g I'll just about guarantee it everytime...

Next, there is a dream about the OPTIMIZED SRV, where the bad li'l spice
steals the Farmers oxy-acetylene torch and clamps a hose on the end (w/
about 5 clamps) makes sure only 02 is flowing, takes the CORE out of the
tire valve, clamps on to it, and uses 1 g of Pd to 100 g alkene, per Os,
and that,

we shall be reporting....

--------------------------------------------------------------------------