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Author Topic: morphine sulfate >> diacetyl  (Read 119 times)

tryl

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morphine sulfate >> diacetyl
« on: June 16, 2011, 10:42:10 AM »
i have a bit of a suspicion this might come off a bit retarded by this board's standards, but well, here goes.

SWIM has access to morphine sulfate caps, the kind you empty in your cooker, dissolve the grains, wait for the paraffin to crust, and pull a pretty clear, readily slammable morphine sulfate solution (it's a maintenance program, along with methadone this, where i am located at in eastern europe).

SWIM also happens to have a bottle of acetyl chloride lying around.

SWIM also did already successfully convert once, but suspect unnecessary yield loss.

so SWIM wonders what's the best way to go about this.

SWIM thought the sulfate, just like the base or any other salt, was readily acetylated, but most sources (admittedly semi-informed junkie know-hows) claimed otherwise - that the sulfate needs to be freebased using baking soda and from thereon acetylated.
well, in the rush, and just to be on the safe side (though not himself convinced sodium bicarb would cleave the sulfate, and that this is necessary at all), he did add (perhaps a bit much) baking soda and heated till left with white powder. as said, it did overall work, but SWIM is unsure of the theoretical yield of such a reaction to start with, and 200mg morphine didn't seem to produce a very satisfying yield.

so, again, is the salt-base conversion really necessary?
and would it be more effective to, say, just add a NaOH solution (pH?) dropwise till the crystals fall off?

and what about the % yield?
"In the words of Archimedes, give me a lever long enough and a place to rest it... or I shall kill one hostage every hour."

POSEIDON

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Re: morphine sulfate >> diacetyl
« Reply #1 on: June 16, 2011, 12:48:57 PM »
SWIM also happens to have a bottle of acetyl chloride lying around.

http://en.wikipedia.org/wiki/Acetyl_chloride
Frequently such acylations are carried out in the presence of a base such as pyridine, triethylamine, or DMAP, which as catalysts help to promote the reaction and as bases neutralize the resulting HCl. Such reactions will often proceed via ketene.

Swim have a bottle of pyridine?

UTFSE MORE dont be lazy
The chemists are a strange class of mortals, impelled by an almost insane impulse to seek their pleasures amid smoke and vapour, soot and flame, poisons and poverty; yet among all these evils I seem to live so sweetly that may I die if I were to change places with the Persian king.
— Johann Joachim

tryl

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Re: morphine sulfate >> diacetyl
« Reply #2 on: June 16, 2011, 01:05:17 PM »
i think i'll just skip on the catalyst, im content with whatever % monoacetyl there is left.
"In the words of Archimedes, give me a lever long enough and a place to rest it... or I shall kill one hostage every hour."

Balkan Bonehead

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Re: morphine sulfate >> diacetyl
« Reply #3 on: June 16, 2011, 07:03:39 PM »
Ja, you should have an acid scavanger. Try sodium carbonate if you don't happen to have a bottle of tertiary amine lying around. It is better than nothing.

jon

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Re: morphine sulfate >> diacetyl
« Reply #4 on: June 16, 2011, 08:41:35 PM »
even with anhydrides using sodium acetate greatly speeds things up.
i would use a little sodium carbonate.
but wait you said you were on maintenence?
why would you want to use heroin again?
sort of defeats the purpose does'nt it?
« Last Edit: June 16, 2011, 08:44:24 PM by jon »

POSEIDON

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Re: morphine sulfate >> diacetyl
« Reply #5 on: June 17, 2011, 12:51:03 AM »
The chemists are a strange class of mortals, impelled by an almost insane impulse to seek their pleasures amid smoke and vapour, soot and flame, poisons and poverty; yet among all these evils I seem to live so sweetly that may I die if I were to change places with the Persian king.
— Johann Joachim

jon

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Re: morphine sulfate >> diacetyl
« Reply #6 on: June 17, 2011, 01:41:51 AM »
i would freebase it and solve it in toulene then acylate it with a little sodium carbonate stirring should do the trick.
making heroin aint rocket science.
i know some others who will tell you the same.
i've done it in glacial acetic acid
so many ways to make heroin

tryl

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Re: morphine sulfate >> diacetyl
« Reply #7 on: June 17, 2011, 05:46:41 AM »
yea, i know, as i said, i've done it - but the yields weren't as satisfying as i thought they should have.
i know about sodium acetate and been considering it, but my chems are locked in the basement and my mom has the keys... long story.

i am not on maintenance, i am not even hooked, a friend is.

anyway..
"In the words of Archimedes, give me a lever long enough and a place to rest it... or I shall kill one hostage every hour."

tryl

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Re: morphine sulfate >> diacetyl
« Reply #8 on: June 17, 2011, 06:33:02 AM »
wait, glacial acetic acid?

what would that give you?

halfway acetylated smack?

6MAM?
"In the words of Archimedes, give me a lever long enough and a place to rest it... or I shall kill one hostage every hour."

tryl

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Re: morphine sulfate >> diacetyl
« Reply #9 on: June 17, 2011, 06:36:28 AM »
also, what is the theoretical yield?

anyone?

i seem to get something like 50%...

which is still not too bad, but i believe it could be around 80%.. i might be mistaken.

and carbonate is a better option than bicarbonate i take it then?
"In the words of Archimedes, give me a lever long enough and a place to rest it... or I shall kill one hostage every hour."

Enkidu

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Re: morphine sulfate >> diacetyl
« Reply #10 on: June 17, 2011, 09:21:00 AM »
If you want to discuss the acylation of morphine with acetyl chloride, at least post a representative acylation procedure of aryl and alkyl hydroxyl groups. Reaction conditions, solvent, salt vs. base, etc should be discussed instead of 'this one time I mixed this with that.'
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