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Recrystallizing with n-Heptane Options
 
nigl
#1 Posted : 10/4/2012 5:19:21 PM

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Hello,

I happened to come across some high purity (HPLC grade) n-Heptane. Has anyone ever tried to recrystallize their DMT with pure n-Heptane or just bestine (mixture of heptane isomers).
I will try nevertheless but previous experiences would help a lot.

Thanks
 

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endlessness
#2 Posted : 10/4/2012 5:20:45 PM

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Works just as well.
 
nigl
#3 Posted : 10/18/2012 5:52:35 PM

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Hi,

I wanna post my results + procedure in this thread as well.

I started off with about 1.2g of STB-extracted DMT:


I put it in an Erlenmeyer-flask and dissolved it by heating it in HPLC grade n-Heptane while vigorously stirring with a spatula.
After all was dissolved a small orange spot appeared on the bottom of the flask, this could be oils or something else which is quite probably NOT DMT so I decided to filter it off:



I added ~1g of activated charcoal and stirred while keeping the solution hot in order to avoid precipitation.



After ~5 min I filtered the solution. You should filter at least 2-3 times because charcoal will come through the filter. I was an idiot and just filtered once which led to problems later on.



After that you can see that the solution is much clearer (the yellow oils/dyes have been removed by adsorption on the charcoal). I then proceeded to boil off some of the Heptane until the solution gets cloudy while boiling.



After that I added just a 1ml of fresh heptane to make the solution go clear again and then I poured all in an crystallizing dish.



I'm going to let it cool now and will report back tomorrow or so when I collect the crystals.

PS: I said before that I had problems because of too little filtering: When the solution became cloudy I saw that little black stuff was still floating around so I had to dilute the solution again, filter, and then let it boil off again which was a huge pain because it precipitated in the filter and a needed a lot of solvent to get it out.
 
nigl
#4 Posted : 10/20/2012 10:57:37 AM

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Here are the crystals I got, strangely enough there is some yellow stuff still around. I will keep that separated from the rest to purify it once again in the future I think.

 
Purges
#5 Posted : 10/20/2012 12:57:10 PM

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Looks much like the result of converting Fumarates to freebase using water precip and sodium carbonate. Bet you its extremely potent Drool
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nigl
#6 Posted : 10/31/2012 6:38:50 PM

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Another one just for fun, didn't get rid of all the yellow but the crystals are nice

 
MMPA
#7 Posted : 11/26/2012 11:49:12 AM

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Very nice job.
 
Orion
#8 Posted : 11/26/2012 1:18:02 PM

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Some very nice formations nigl. You may want to consider reducing pictures down to around 1000 pixels just to speed up the thread for folks Thumbs up
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The Traveler
#9 Posted : 11/26/2012 1:32:40 PM

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Orion wrote:
You may want to consider reducing pictures down to around 1000 pixels just to speed up the thread for folks Thumbs up

Agreed, if you attach the images to your post then they will automatically be resized for the forum. If people still want to get the original pictures they can click on the scaled down images to download the full version of it.

Also note that .jpg files that are uploaded to the forum are automatically stripped of their EXIF header to protect your privacy!


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