where/how would I find/make

a) propyl iodide
b) CH2Cl2
c) acetic anhydride (can I just boil acetic
acid?)
d) Hunig's base (diisopropylethylamine)
e) Diethyl ether

?

a) you need to either react HI with n-propanol which you will have to get from a chem supply or react an excess of propane with iodine in a glass vessel with light, Both of these are quite difficult.
b)DCM not suspicious if ordered from a chemical supply but it can be distilled from certain furniture strippers.
c)acetic anhydride can be made with sodium acetate and acetyl chloride, acetyl chloride can be made from phosphorus trichloride and acetic acid, so the easiest yet more deadly way to make it involves the pyrolysis of acetone to form ketene and then dissolving the ketene in glacial acetic acid thus forming acetic anhydride. Note that ketene bubbled through water produces acetic acid so you could just start with high concentration acetic acid or distilled water.
d)ethylamine reacted with two equivalents (preferably more) of isopropyl halide (not chloro)
e) You can distill it out of starting fluid, but you will need lots of ice or a dry ice/acetone condenser. If you have large cohojnes or the experience you can distill it out of a mixture of 95% sulphuric acid and ethanol. but it might just be best to get this from a chemical supplier.

None of these are really easy to get except maybe the DCM.

quote:

---

Originally posted by tryptamine:
e) You can distill it out of starting fluid, but you will need lots of ice or a dry ice/acetone condenser. If you have large cohojnes or the experience you can distill it out of a mixture of 95% sulphuric acid and ethanol. but it might just be best to get this from a chemical supplier.

---

diethyl-ether is a non polar solvent. it floats on top of water. starting fluid sprayed in a jar filled 25% w/ water. cant you get it that way? thats always how i have.

Starting fluid is a mixture of ethyl ether and hexane/petroleum ether. If you mix the contents of the can with water the hexane(which is very non-polar) will all be separate and some of the diethyl ether that you want gets sucked into the water as it is slightly soluble in it. And the rest of the ether stays with the hexane.

Essentially by using this water method you are throwing away good ether and not getting rid of the hexane.

Can't acetic anhydride and diethyl ether be
made from ethanoic acid and ethanol by
dehydration (i.e. boiling the water off, lack
of H2O would disturb the equilibrium causing
dehydration synthesis to occur)?

And is L-tryptophan illegal (now that would
be silly, since we need it to live)?

Di ethyl ether is made from ethanol by dehydration. However becase dehydration requires some very tortuous conditions you can't simply heat the stuff and expect it to form. You need a strong dehydrating agent. Concentrated sulphuric acid is what is used industrially. It rips the water out of the alcohol. This is what I described in the original post.

Acetic anhydride cannot be made in this way, there is no practical way to dehydrate acetic acid. You need to use ketene period.

L-tryptophan is banned by the FDA because years ago an impure batch was imported and caused several deaths. By the time they found out and corrected the toxic impurity the supplement was made illegal for human use (animals can still get it) Strangely the natural protein(which we eat every day) that has anti-deppressant activity was banned around the time that prozac was released?????? Hmm funny how our laws work...

I mean come on tryptophan is found in any meat product and most grains and plants yet it is banned as a supplement because it is toxic. I think our archaic laws should be re vamped... Fucking beaurocratic shitheads.

Ah damnit, stupid government.

What about indole?

Indole is extremely difficult for the average bro to get due to the fact that no one really needs it. Just get animal grade tryptophan.

Now if one were to, hypothetically, find himself in possession of 500ml of acetic anhydride, of what use would it be?

[I know what it's theoretically used for, I mean what theoretical good would it do someone who has no intention of using it like that and knows nobody who might?]

Acetic anhydride can also be made from vinegar. Household vinegar is mixed with NaOH until nuetral, then all water is distilled off. The remaining Sodium acetate is reacted with conc. sulfuric acid to make conc. acetic acid and sodium sulfate. The acetic acid is distilled. Then sulfuric acid is reacted with NaOH until nuetral, and all H2O is distilled off. The reamining sodium sulfate is placed into a glass gassing apparatus, and heated to about 250-270 degrees celcius, it breaks down and forms sulfur dioxide gas. This is bubbled through the conc. acetic acid to get acetic anhydride/acetic acid mixture.

Tanks for that mad I didn't know about that technique, there are easier ways of getting SO2 BTW. Use the sodium sulphate from the first reaction in the last one too.

Rev for acetylating things like morphine --> Heroin. Also one of the steps in making ludes requires it, making GAA from 90% Acetic acid, All sorts of other things.

I was more interested in DPT, but yeah it is
used for making heroin (I wonder why regular
CH2CO2H can't be used for it though).

Because the water leaving group that must be removed if one wants to acetylate the phenols on morphine needs some help. So ya gotta use AA. What is the acetic anhydride used for in the DPT synth?

I'm reading the synthesis out of shulgin.

I can't see the purpose, here's the breakdown
of the procedure:

1) tryptamine base in 2-propanol is treated
with propyl iodide and hunig's base (NaHCO3
can also be used but reduces yield 5 fold)

2) volatiles removed

3) residue partitioned between CH2Cl2 and
NaOH(aq) (I have no idea what this means

4) residue treated with (CH3CO)2O and heated
in steam bath.

5) Cooled, small amount of NH3(aq) added and
mixture added to H2SO4

6) washed 3 times with CH2Cl2 and made basic
with NaOH

7) extracted with CH2Cl2, pooled, solvent
removed.

8) results in N,N-dipropyltryptamine freebase
oil.

Steps to form salt skipped.

I know there are probably reagents and solvents
that could be substituted, and ways to do
it differently, but I wanted to consult
yous guys.

Hmmm good thing I only lent out my PIHKAL over the Christmas holidays and not my TIHKAL.

Ussually Shulguins descriptions of his procedures are a little more detailed in why he does what and in describing the intermediates this one is a little vague.

The acetic anhydride is added presumably to decompose the quaternary ammonium salt into the tertiary amine(our desired product). I say presumably because I am not sure.

You may be able to use another base like ammonium acetate or any number of tertiary amines and still get a decent yield.

Oh yeah and the partitioning step step 3 what he is doing is disolving the residue in water and bassifying with NaOH, then extracting into DCM several times(washing with DCM). Except he just makes up the two solutions and then just dumps it in all at once.

I'll have to check some of my sources (it may have been DiPT I saw), but I'm pretty sure DPT is readily available. Why don't you just buy it?