Author Topic: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg  (Read 6377 times)

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bizwax

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Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #20 on: August 09, 2000, 09:26:00 PM »
Check Rhodiums page under "Osmium's variation of the Al/Hg reductive amination of MDP2P" concerning EtOH and IPA.

frost

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #21 on: August 11, 2000, 05:34:00 PM »
mm,
great write up! drx has done the benzo with formamide but not with meoh. 1 question is the heating absolutely necessary when the reaction is 80% complete? swim thought that this was an exothermic reaction after 4 1/2 hours, does the meoh use over mdf or formamide make for the heat requirement or could dr x just let it go for an hour or two more?
thanks in advance!
frost

Cheeseboy

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #22 on: September 06, 2000, 03:20:00 PM »
Can the Toluene/product layer be extracted using aqueous HCL and dh20, like instead of gassing? You know , like in methead's speed synth? Or is that route only OK for Speed? And does gassing give you better yields than extracting with aqueous HCL & dh2o?


!

jinx71

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #23 on: April 05, 2001, 01:02:00 PM »
sup,
In step #19 of the amination, u state the following:

   19. Wash the toluene/product 4 times (or more) in your sep funnel with 400 or 500mL H2O and a final time with 500mL of a saturated NaCl solution to remove any traces of solvated HgCl2.

Can you bee a little more specific about the "saturated NaCl solution? Maybe how you made it, %'s,  etc.

Also, after the "spike" you say that a little heat can be added but stopped 30 mins prior to finishing. How much heat?

 

I'm out.

jinx71

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #24 on: April 05, 2001, 01:24:00 PM »
Thanx MadMax,

That makes perfect sense. Any suggestions on locale of NaCl?
Any precautions that need to be taken?

Later

yellowjacket

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #25 on: April 05, 2001, 01:55:00 PM »
NaCl, also known as sodium chloride, can only be found in the center of black holes. It has unique anti-gravimetric tachyonic wavelet properties that can cause inverse subspace distortions, so be sure to wear saftey glasses.


marijuana is the flame, heroin is the fuse, LSD is the bomb!

jinx71

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #26 on: April 05, 2001, 02:38:00 PM »
Gee thanx yellowjacket,
   
    alot of useful info could have been spewed by you in those 3-4 sentences but NO....gotta be a smartass huh? Hey, i'm just a squirrel tryin to get a nut, that's all.  At least MadMax knows what time it is.

Later,





RollWitMe

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #27 on: April 05, 2001, 02:52:00 PM »
But yellowjacket, once you get the NaCl in the center of the blackhole, how are you supposed to get back to your lab? Or for that matter, back to your kitchen table to put some on your chicken or something. I guess I should bring my plasma spraying transmogrifier so I can warp back to planet "shoot me in the head if someone asks me what NaCl is."  Just a thought, though, I really have no idea how to get back with the salt. :(


I like to cook!

riobard

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #28 on: April 05, 2001, 04:46:00 PM »
BWahahahahahhah! someone give that guy a nobel prize for figuring out how to navigate singularities. That's assuming he can make it back to this saltless planet. ;D

DiethylEtherMan

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #29 on: April 05, 2001, 11:06:00 PM »
jinx:

yea...no additives. In my experience, pickling salts usually has no additives.

And add enough heat so that the meoh mixture is mildly refluxing when the addition is 80% finished. My mother has done it with really no heat, and the only drawback is a horrible mess during the extractions. Lots of al will stay un-broken down (if thats a word) if you do not reflux (use heat).

Good Luck!


If some of us were not so far ahead, the rest of you would not be so far behind!

weasil

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #30 on: April 06, 2001, 01:38:00 AM »
When you add the methanol + nitro to the ketone (preaddn) is the soln almost colorless? New ketone was aqua marine rather than greenish yellow. It almost had a blue tone to it in addn to the green.
Upon basifying does the soln turn yellow/green?
The last time did this reaction failed (same thing happened as did to noj; used photostore PdCl2 suspected problem)
This time using Laboratory grade PdCl2 so hope this fixes it.
Obviously am a bit skeptical since never had success. Will post results though in a few hours.

legion

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #31 on: April 06, 2001, 02:03:00 AM »
Just trying to make sure I'm clear on this one. Someone else has asked this already but as I am still in my reading and learning phase, I need to be sure I understand.

......
7. Extract flooded mixture with 3 portions of DCM (1 x 500mL, 1 x 250mL, 1 x 100mL) in a large separatory funnel.  The desired raw product, MDP-2-P (“ketone”), migrates into the DCM as an oil.  Separate the DCM/ketone layers and combine them.
(Note: when you first hit it with the DCM you will probably observe a bit of scum which will float on top of the water layer, which will work its way down during these three extractions to appear as a blob of spongy semi-solid interface.  It’s actually very mobile and easy to work around; simply avoid allowing it into your DCM separations.  The same thing will happen in your washes in steps 10, 11 and 12 below, but by then you will be quite the pro at working with it.)
8. Extract water layer with a final small amount of DCM.
9. Add this final small DCM extraction to the combined oil/DCM solution from step 8.
......

Step 8. How can you extract the water with DCM when DCM extracts oils. Should that be "extract with a final small amount of DCM" ? Whats this about the water layer ? As I understand it, presumably you could wash the water layer of all its ketone goodness with the DCM, but whats the point in keeping the washed water layer ? Why do we all of a sudden want some of the water layer ? Also on step 9, should that be corrected to "Add it to the combined extractions from Step 7" (and not 8) ?

please can someone clarify this for me.

muchas gracias

spric

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #32 on: April 06, 2001, 09:47:00 AM »
You are thinking too hard buddy.  You are extracting stuff out of the water.  it doesn't make any sense to extract water from an aqueous layer.  and jinx/saltman, i am sorry for giving you some help before.  If you have to ask these types of questions, you will hurt yourself in  your lab.  You are also going to waste quite a bit of your money.  MDMA is a relatively simple synthesis.  And for you weasil (sorry, nothing bad to say yet), was your ketone blue before addition.  Blue ketone seems to be made when the sassy is not distilled properly.  and after the almagation you basify and it turns yellow?  wierd.  Does your ketone smell like lemon lime kool aid with a hint of latex?


Information is Not Knowledge

weasil

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #33 on: April 06, 2001, 10:20:00 AM »
Wusup, basically I doubted you dudes but you’re sheet backed up with decent references so I think that something else must be to blame. Basically someone had yielded methanolic Benzo yields of ketone. Threw the first one out because amalgamation was identical to what noj was complaining about. Anyway on the second lot of ketone trying to follow MM to the T cept using thicker foil. NXt day tried extracting with toluene but toluene is greenish/silver. Know you will say all ketone didn’t react but it was in the flask right from the start so wood af had nuff time. Serious problem aight. This didn’t clear after washing with water (starting to think fuck washing this shit). Noticed white crystalline mass between layers but this was excluded from extract. (Know what you are thinking but how can Xtals form if product ha not been gassed yet). After gassing and adding HCl no product is visible. WTF?. One time is bad enough but spending 2K I expect yield just like you wood. Sorry to report shit, but you would be feeling like me if you did same ting. If you saw mw do this now you would accept that could not have done wrong ting ya, represent. Either photo shop Benzo or NaOH drain cleaner to blame now. I have been through the pain shed my tears. But now my evil is purer than ever so I am ready to synth killer reaction. Will order 40% MeAm soln despite what u say, will do OS version. If Ketone is pure then expect KILLER yields, for real. No interference. Yes no fear, I am tragically saddened by this madness. Toluene was put in screw top bottle and 35% HCl was added. This was placed in Freezer and still no Xtals!. How many times did other guyz fail before success. If I kill someone for my pain then this shit will bee worth whilw, so that is my aim. Flatliners be'ach. By the way is there any way someone can extract eh goods from the water wahed aluminium mess. If so I would like to know.

jinx71

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #34 on: April 06, 2001, 11:46:00 AM »
sup,

Hey pric.... oops!(spric), there's no need to bee like that. Would you rather newbees ask no questions and make tons of assumptions on the threads that we read. Dude, bees ask questions, they learn to make honey.....not asking is how bees hurt themselves. I've asked some seemingly dumb questions i'm sure we all have , but only in the search for knowledge. I played pro ball for 6 yrs, chemistry was not top of the list in college (beer and bitches ranked alittle higher), so bare with me if some questions seem elementary. It's all the wonderful input and knowledge that i have gained at the Hive that keeps me coming back, obviously for you it's something different. Not all of us where born with the know-how  from birth, some of us have to learn BY ASKING FUCKING QUESTIONS. besides, if it weren't for the better half telling me to get a hobby(hehehehe), this would've been avoided. I would prefer to watch my portfolio drop another $300,000 than to read one more post with an "expert" doggin on a newbee for asking a damn question!
Most everyone knows where the search engine is and how to use it, it's just that most of the shit is buried in a bunch of jibber-jabber, why do u think the same questions keep coming up? All you're doing by flaming fools is discouraging them from posting. That seems more dangerous than anything IMHO.



DiethylEtherMan

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #35 on: April 06, 2001, 11:49:00 AM »
Weasil:

I have experienced blueish (or dark green) ketone before and have got to the end with fine results. As spric says, I think the weird color is a product of not distilling the safrole well enough. I know I told you this before, bro, but for me it was the sassafras. bad sassafras. And, from what I have been told, so was noj's. He got a little sample of REAL sassafras from a source who knew it was REAL from his own attempts and all of a sudden, his reaction worked. So, ask him. If you have the tone dude, even with semi-bad benzo, you should at least get some product. I have used dirt brown benzo and still got great results.

Also, in my experience, when the toulene is dis-colored and not foggy white...your fucked. Its bad tone, or not tone at all. I have experienced this many times. Your toulene should be foggy white even during the washes, up until you dry it with mag sulfate. After you filter the mag sulfate, toulene should be clear as day. (i don't know why, but it is, at least, in my experiences)

Of course, I am not sure if you have the same problem as I initially did (bad sassafras), but I'll tell you that it was the last fuckin thing I changed (success finally!), which really pissed me off because by that point I had wasted mega $$ and tons of chems. I thought it was this and that...and it was the sassafras. The al/hg is very forgiving so when you talk about bad benzo and pdcl2 or bad NaOH...I think you just trying to fix the wrong problems. Just for the fuck of it man, I would try a different batch of sassafras. But its up to you, of course.

Good Luck.


If some of us were not so far ahead, the rest of you would not be so far behind!

weasil

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #36 on: April 06, 2001, 11:51:00 AM »
Chill kidd, you r new to this game. The hive is about pain. If you are not feeling pain yet then have not done uyet nearly enuff reasesrch. Comeback and ask questions when you have becone nasty.

legion

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #37 on: April 07, 2001, 10:54:00 AM »
right I'm fucking nasty. If I'm not missing something then why doesn't MM just say to do four extractions at Step 7 instead of saying do three, then to do another one again but telling to "extract the water layer". Remember I havn't seen a fucking RB flask yet so I'm getting this all straight in my head while I wait for the shit to come together.

later

spric

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #38 on: April 07, 2001, 05:26:00 PM »
I did not assume I was an expert.  I failed at first too, and it makes you feel really pissed off.  What I said is the fucking truth.  When you are done with your frat party, you may realize that this shit can be physically dangerous.  Even a 2L flask full of solvent can make quite a bonfire.  Once you get sulfuric acid in your eye, I will  bee willing to accept all of the shit you spew.  It's like all of those cooks without any chemistry experience with those burn marks all over their body, or maybee you have never met any.  When you ask a question that elementary, you set yourself up for the jokes.  I've been flamed for fucking posting a zinc borohydride reduction that I never myself tried, so get used to it you salty dog.
And from one pric to another, good luck.

Oh yeah, if it was your benzo, that is that the benzo is complete shit, you will get about 5% of the expected yield.  If you are worried about your NaOH, go to the hardware store and buy a bag of caustic soda for you septic tank, it is of decent purity and a 50lb bag costs thirty bucks.


Information is Not Knowledge

baalchemist

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #39 on: April 11, 2001, 03:15:00 AM »
Most of the time failures newbee failures are due to lack of comprehension of the functions of each step. Which is no surprise as most are not chemists. Thats why its important to understand everything 100% before going at it. Baal studied this shit for over a year before going at it, for personal & public safety. Success 1st time around, but couldnt crystallize shit for 6 mos. Ended up with a big damn jar of E-base, and a head full of frustration. Put chemistry away for 3 mos,studied,came back and crystallized that jar of base. Patience & persistance are ones best tools, if chemistry's your bag. Things are very relative with chemistry    lack of knowledge=big economic losses