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21796.14 Points
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dimethyl-holafébrine
Sun Feb 13, 2005 9:21 am |
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apis
(Stranger)
06-06-00 19:04
No 14429
I want to make it bigger. Bookmark
O Thou, mighty elephant headed god of experience, clearer of obstacles and beneficent guide of the ignorant and cocky: What do I need to know to safely and productively upscale a reaction of this nature (say, 300x) ?
Would this reaction work with acetone instead of formaldehyde to isopropylate an amine?
Tet. Lett. 3, 261 1973. B. L. Sondengam
Formaline (35%, 35 mmol) was added with stirring to a solution of holafébrine
(prim. amine) 3 mmol in methanol (10 ml) and the solution was refluxed for
30 min. After cooling 400 mg NaBH4 was added slowly. After 1 h the reaction was
evaporated and the mixture was extracted with CHCl2. Evaporation yields iréhine
(dimethyl-holafébrine, 85%).
I bow down to your exquisitely manicured toenails in advance. thankyou
Rhodium
(Chief Bee)
06-06-00 19:20
No 14435
Re: I want to make it bigger. Bookmark
1) First, try it out on a 5-10 gram scale to see if it works satisfactorily.
2) The only things I can think of with the scaling is that you probably do not need to scale the solvent 300x, try 150x and see if all the amine dissolves first. Also, you need good cooling, and make sure that the NaBH4 additions doesn't cause too much foaming/heat when you add it. You are scaling the heat evolution 300x, you know.
3) If it works satisfactorily on the tryptamine of your choice, please give a full report on your procedure and yield to me, and I'll upload it to my page.
http://rhodium.lycaeum.org
Vulpes
(Stranger)
06-07-00 11:33
No 14803
Re: I want to make it bigger. Bookmark
Apis could you mail me at red_fox@hushmail...
Lilienthal
(Moderator)
06-07-00 12:55
No 14832
Re: I want to make it bigger. Bookmark
Try it with < 50 mg. But the most important thing is: check the reaction by TLC if it takes the right way and how fast. Do not even think of starting this reaction without TLC equipment and reference substances. This type of reaction is not really tested with tryptamines. Tryptamines with formaldehyde cyclize under H+ catalysis into beta-carbolines (Pictet-Spengler-Reaction). Please post your results (positive as well as negative ones) since we are highly interested in that.
Rhodium
(Chief Bee)
06-07-00 13:20
No 14841
Re: I want to make it bigger. Bookmark
I have a post from KrZ on my page where he makes DMT from tryptamine in moderate yields using NaBH3CN (and he even added some acetic acid to the mix)...
http://rhodium.lycaeum.org
ScuzZ
(Hive Bee)
07-03-00 06:13
No 24122
Re: I want to make it bigger. Bookmark
Dude, in attempting this reaction. I give you one part of advice.
Whenever heating acetone make sure you heat it steadily and never let the temperature drop to dramatically otherwise you'll never have the arms to post another message.
Rhodium
(Chief Bee)
07-04-00 16:52
No 24641
Re: I want to make it bigger. Bookmark
Scuzz: I don't agree with you on that, and this doesn't apply to the reaction above anyhow, as acetone is just a reagent, not a solvent (methanol is).
http://rhodium.lycaeum.org
ScuzZ
(Hive Bee)
07-05-00 19:27
No 25125
Re: I want to make it bigger. Bookmark
You know what I mean dude. I was just a little wacked when I wrote it.
eli3
(Stranger)
07-08-00 04:55
No 26079
Re: I want to make it bigger. Bookmark
yes,yes we "know what you mean"(wink,wink,nudge,nudge);know what you mean...
you mean, YOU DON'T KNOW A GOD DAMNED THING ABOUT CHEMISTRY.(or possibly anything else since you can't even lie worth a shit!)
Try again!
"pull the wool over your own eyes"
eli3
(Stranger)
07-08-00 05:03
No 26081
Re: I want to make it bigger. Bookmark
oh yeah, now i remember, the old "acetone arm explodie trick"; thats a good one...
have you been trepanned?
"pull the wool over your own eyes"
eli3
(Stranger)
07-08-00 05:25
No 26089
Re: I want to make it bigger. Bookmark
Rhodium, can you think of any drugs that lobotomize the user, leaving them unable to speak or write(think?) a word of rationale?
lode me up......i want to get "whacked out".
"pull the wool over your own eyes"
Rhodium
(Chief Bee)
07-08-00 12:02
No 26223
Re: I want to make it bigger. Bookmark
eli3: No personal attacks in this forum. We have private messaging for that.
http://rhodium.lycaeum.org
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