02-10-03 12:12
No 406289
After lurking around here & Rhodium's site for a few years, slowly & patiently gathering knowledge (so much farther to go), equipment & chems swim is ready to try the methadone synthesis Rhodium worked so hard on. A few questions first; In the "Introduction" of the write up it states that 2,2-diphenyl-4-dimethylaminovaleronitril
(Chief Bee)
02-10-03 15:13
No 406380
The structural formulas for the nitriles are drawn in the document, and their molecular weights are identical, as they are isomers. The exact molecular weight can be had by counting the atoms and multiply with their respective atomic weights. If that is too complicated, you can make use of the calculator at https://www.the-hive.ws/forum/pt.pl?Cat=
You can either scale the precursor preparation up or the methadone synthesis down depending on how much product you aim for.
If I have made a mistake in the introduction part, I'll fix that.
(Stranger)
02-11-03 04:04
No 406626
Chieftain, Thank you for your quick reply. Swim is still learning how to decipher chemical sturctures, though as swim asked you pointed swim in the right direction. Swim can not thank you enough for all your hard work with the methadone write up. For a little more than 1 month's fee at a maintenance clinic swim purchased enough of the two precursors to make a few years worth of product and now can tame the brown sugar habit. Thanks again.
(Hive Addict)
02-11-03 04:17
No 406633
if you are talking about the methadone synthesis:
../rhodium /methado
including the synthesis of all precursors, and this is
your first attempt at organic chemistry, then consider
to start with a much simpler syntheses.
most of the reagents in this synthesis could be invested into
simpler / more worthwhile compounds.
for example mandelonitrile can be turned into speed in three steps.
if you want to handle metal organyls, look into phencyclidines.
if you want an opiate, how about exctracting / acetylating morphine?
etc, etc...
(Stranger)
02-11-03 06:34
No 406665
Before acetylating morphine swim wants to have something to help control the monkey. Swim already has the 2 main precursors in reagent grade for methadone. It is amazing what you can find if you look. As for the mol weight of the nitrile swim believes it is 278.40.
(Hive Addict)
02-11-03 07:08
No 406682
so you plan to make heroin, indeed so much of it as to get physically
and mentally addicted to it, so before you even start making h, you make
methadone, which will help you through the turkey. sounds strange to me,
but why not!
(what about making h and trading for methadone?)
(Chief Bee)
02-11-03 17:05
No 406840
Toltech: You got the molecular weight right.
(Hive Bee)
02-12-03 16:09
No 407212
I obviously cannot be certian how serious you are about making H/Methadone but I would suggest if you plan on getting addicted to H then maybe you should not start. According to Boroughs (sp) it takes about a month of straight H to get really addicted, and I wouldn't rely on the methadone to save you.
Just something to keep in mind.
(Stranger)
02-13-03 04:34
No 407368
I appreciate the concern. Swim is not going to synth something up in order to become an addict. Swim already enjoys the "junk". Swim wants to take a break from swim's "brown sugar baby" habit but does not want to get dope-sick ever again or pay the ridiculous cost of methadone maintenance. Anyway this thread was started asking for help on this procedure.
(Stranger)
02-13-03 12:24
No 407477
If I should enter this in another thread please let me know. I am now trying to learn about stoichiometry,writing and balancing equations, determining limiting reagents, and the math to do this on my own. Progress is slow but I am learning. Anyway while preparing to write out and balance the equation for method 1 of the nitrile synth in ../rhodium /methado
Can I move the decimal point in the mol calculations one place in the same direction for each compound? So the above mentioned example would then read; "A suspension of 13.59g (0.34 mol) of finely ground sodium hydroxide was prepared in 10 ml of dried DMF. A solution containing 59.9g (0.31 mol) of diphenylacetonitrile in 8 ml of DMF was added thereto at room temperature. After stirring the mixture for 15 minutes, 53.74g (0.34 mol) of 1-dimethylamino-2-chloropropane were added. The reaction mixture was heated with stirring to about 50°C for about 1.5 hours and was then cooled.........etc..." Would this keep the ratios similar. Also how do I determine by how much to change the quantity of solvents used? All replies welcome. Please view the write-up at ../rhodium /methado
(Chief Bee)
02-13-03 14:44
No 407509
1-dimethylamino-2-chloropropane is C5H12ClN with a mw of 121.61 - you have a chlorine atom too much. If you look at the structures on my page, you see that the "2" signifies the placement of the chlorine atom, not that it would be two of them.
Can I move the decimal point in the mol calculations one place in the same direction for each compound?
Yes, to scale up or down, just multiply every weight and volume (both reactants and solvents) with 10 or 0.1 depending on if you want to scale up or down. Temperatures and reaction times stays the same. If scaling up 10x, perhaps you could cut back on the solvents with 25% or so, and if you scale down, use 25% more than calculated.
(Stranger)
02-14-03 13:12
No 407885
Chieftain, Thank you so very much for your help! From your website to the writeup; ../rhodium /methado
(Stranger)
04-08-03 04:07
No 424734
I believe I have made a mistake and overlooked a very important item. Swim was only able to aquire 1-dimethylamino-2-chloropropane hydrochloride which I now realize has a mol weight of 158. If I am now correct what needs to happen is that this hydrochloride needs to bee turned into the freebase form for this procedure to work; ../rhodium /methado
(Chief Bee)
04-08-03 14:06
No 424840
Correct, you need to use the freebase in the procedure, or use the solventless version where twice the amount of NaOH is used.
The listed method is definitely the easiest way to produce clean freebase, it might also work without the final distillation, if the freebase is not colored after drying it over some NaOH pellets until it's not cloudy anymore.
(Stranger)
04-09-03 03:57
No 425049
Thank you for your help! Swim will write again.
(Stranger)
04-14-03 05:30
No 426590
Swim was able to make the freebase of 1-dimethylamino-2-chloropropane. It stayed an oil with a seeming emulsion below it after separating it from the NaOH mix. Swim tried extracting with anhydrous ethyl ether but did not realize the low boiling point of the freebase until the dish was all but empty. So swim "created" the freebase again & used the oil. Heating & cooling in hexane left about half of what was put in so I assumed it worked though I do not have melting point equipment. Swim also failed to research Grignard reactions & tried the 2nd method for methadone listed in ../rhodium /methado
(Chief Bee)
04-15-03 05:41
No 426941
Almost all grignards look the same when initiated - they heat up and the magnesium begins to be consumed. UTFSE on "grignard initiation".
(HyperLab Bee)
04-17-03 04:23
No 427559
1. For preparing of nitrile try to make PTC reaction like in Patent US4242274. In this method you can use hydrochloride of 1-dimethylamino-2-chloro-propane. It's very simple method. For separation of isomeric nitriles see Patent US2540636 with 91% IPA. You'll get very pure methadone nitrile. For Grignard the best method (high-yielding) is Method 1 from Rhodium's site.
2. How to make Grignard reagent?
1 step. Dry your Mg thoroughly.
2 step. Place Mg in flask, add 2-3 crystals of I2 and heat up the flask until vapours of iodine appear.
3. Cool the flask to room temp.
4. Pour ether in the flask, add approx. 1/10 of EtBr needed and wait the beginning of reaction. If rxn doesn't begin, slightly heat up the flask
5. After rxn has begun, add EtBr dropwise. Ether must slightly boils
That's all.
Good luck
(Stranger)
04-17-03 11:56
No 427619
I'll report back when time permits.
(Stranger)
05-01-03 12:55
No 430652
Swim ran the grignard sucessfully with I2, thanks Murmur, & using method 1 for methadone in ../rhodium /methado
(HyperLab Bee)
05-02-03 03:56
No 430810
Look, man, if you scaled down all reactants, you must scale down HCl too!(quantity not percentage) But in this case add to cold reaction mixture about 500 ml benzene and after few time you'll obtain crude methadone hydrochloride.
For this step see Patent US2601323, Example 3. Next, then you add HCl, don't remove heating, reaction must be very vigorous and all xylene must be removed during addition of HCl.
Good luck, Murmur.