Glacial_Refluxer
(Stranger) 05-22-03 17:37 No 434831 |
Myristicin > MMDA advice needed | Bookmark | ||||||
Swim is vary interested in trying this synth ../rhodium /mmda.ht Can swim use 30% ammonium hydroxide with extended time to aminate or is anhydrous ammonia required? http://www.redcoat.net/pics/arguing.jpg |
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moo (Hive Bee) 05-22-03 18:13 No 434841 |
You need to study chemistry. | Bookmark | ||||||
You need to study chemistry. Don't forget to read PIHKAL either. Screw-ups can cost you a lot more than money and you are going to screw up if you don't know the basics. No offense, because that's the way it is. fear fear hate hate |
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Glacial_Refluxer (Newbee) 05-22-03 18:35 No 434845 |
Thanks but..... | Bookmark | ||||||
Your post did not help at all. PIHKAL synths are a bit more than swim wants to deal with, to many chems involved. So can this amination take place with h2o present? http://www.redcoat.net/pics/arguing.jpg |
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Antibody2 (Hive Addict) 05-22-03 19:09 No 434852 |
Bubble thru 35mL anhydr. | Bookmark | ||||||
Bubble thru 35mL anhydr. MeOH in an ice/salt bath anhydr.=anhydrous=no water you don't want water |
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Rhodium (Chief Bee) 05-22-03 20:07 No 434872 |
My advice: Use another method | Bookmark | ||||||
I thought I had removed that document already, due to the procedure very likely being at least partly bull. I haven't heard of anyone ever successfully repeating that experiment by IudexK, while I get tons of PM's from people asking me to tell them what they did wrong when trying to get any product from it. |
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hypo (Hive Addict) 05-23-03 00:26 No 434912 |
which stepd doesn't work? | Bookmark | ||||||
a friend of a friend ended up with nearly only polimerised crap after doing an performic on iso-myristicin (pump probably too weak), so he is quite interested in this method. do you know which step is bogus? what i'm thinking about is reacting the (fractionated) myristicin with HI in an organic solvent (for example AcOH or DCM?), then recrystallise it. the amination would be done pretty much IudexK style (with magnetic stirring). i figure the big problem here is the production of secondary and higher amines. but phtalimide and hydrazine are not available. is that sound, or should my foaf not waste precursors? |
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Antibody2 (Hive Addict) 05-23-03 05:39 No 434951 |
Hypo-i expect if there were problems it wasn't | Bookmark | ||||||
Hypo-i expect if there were problems it wasn't that reaction(modifiied performic), much more likely too hot a distillation, IMHO. ended up with nearly only polimerised crap after doing an performic on iso-myristicin my sister has seen sucessful performic oxidations of both iso-myristicin and iso-apiole(dill and parsley). In yields that are comparable to what is acheived using safrole. She said if she had it to do again she would do it the same |
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hypo (Hive Addict) 05-23-03 06:18 No 434957 |
yes, | Bookmark | ||||||
i know. that's why i said i think the pump is too weak. the non polimerised fraction came at about 180°C. an oil change is in order... |
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Rhodium (Chief Bee) 05-23-03 16:34 No 435051 |
Amination | Bookmark | ||||||
The most bogus step is very likely the (Delepine) amination... Hexamine amination of a secondary halide is unprecedented in the literature. |
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hypo (Hive Addict) 05-24-03 00:58 No 435122 |
hmm... | Bookmark | ||||||
but note that IudexK is using NH3 in a bomb (sort of). egotrip is using the delepine: ../rhodium /dmmda-2 in the book named after our friend orgy, i read something interesting: "the yield of primary amine can be increased by using an excess of ammonia (obviously) or by adding ammonium carbonate or ammonium chloride" i figure the primary amine being a stronger base will liberate an NH3 molecule and be transformed in the unreactive ammonium ion. the HBr/HI produced in this reaction should already do this to some extent, but having an excess of ammonium can't hurt. nice. |
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Glacial_Refluxer (Newbee) 05-24-03 05:38 No 435160 |
Swim shall give it a try | Bookmark | ||||||
That DMMDA-2 synth looks pretty simple, but swim got kind of discoureged when Rhodium made the comment on the hexamine amination. 2 questions: Swim does not have fractional distill equipment, would useing straight parsley oil yeild anything if the synth is not bogus? Could i2 crystals be used in place of the sodium iodide? http://markmlucas.com/images/invertabrat |
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