The Hive => Methods Discourse => Topic started by: Bubbleplate on September 18, 2002, 04:56:00 AM
Title: Wacker Success! Thanks To All Here!
Post by: Bubbleplate on September 18, 2002, 04:56:00 AM
SWIM had his first sucessful Wacker! Many thanks to all the bees here and Rhodium whose help and postings contributed to the effort. For this dream, 2.5 gm of PdCl2 was used, to "be on the safe side". Yield was 130 gm of the prettiest Antifreeze, with about 10 gm of raw Safrole also coming over. (Man does it take forever to off the dichloromethane!) Two questions: 1) Right before ketone came over, some "snowflake" shaped white crystals came into the stillhead. Was this benzoQ or something else? 2)SWIM isn't looking forward to many Hg/Al Reductions at 25 gm. a pop, not to mention the enormous amount of chemical waste and solvent utilization. Has anyone done LiAlH4 Reduction of Ketone or can suggest better Reduction for larger scale? (that you've actually tried)
If they drive God from the earth, we shall shelter Him underground - Dostoevsky
Title: UTFSE
Post by: terbium on September 18, 2002, 05:02:00 AM
Has anyone done LiAlH4 Reduction of Ketone or can suggest better Reduction for larger scale? (that you've actually tried) Yes, sodium borohydride or catalytic hydrogenation, it has all been thoroughly discussed here.
No one (competent) would use LAH for this purpose.
Title: Two words.Osmium and methylamine.
Post by: ChambeRed on September 18, 2002, 05:09:00 AM
Methylamine.HCl ala chromic,al/hg MeAm ala Os. Bee's don't die,we just multiply.Edit:Amination with methylamine has never been done by swic but methylamine.Hcl has been sucessfully prepared using chromics write-up,swic was very pleased with the process itself and yeild doesn't matter much given the starting material,only problem with the whole thing was people at work commenting on swic's peculiar stench for a few days :o that kinda sucked.Peace,Chambered.
Title: slow down tiger.
Post by: RoundBottom on September 18, 2002, 07:35:00 AM
walk before you can run. try a normal scale MM AlHg to see how it works, then, if you have the equipment (eg. a large flask) try a 2x scale MM. then, just for kicks, try to make MeAm, and try an Os AlHg. the more you know, the better understanding you have.
if you think you're going to be pulling 1kg reactions by the end of the year, you'd better think again.
but congrats on getting this far.
my mouth tastes like burning.
Title: IMHO
Post by: SPISSHAK on September 18, 2002, 09:54:00 AM
Catalytic transfer hydrogenation using Palldium on acivated carbon is the best. Methylamine formate is the reageant. Such an eloquent reaction, and the conditions are so mild you can recover your unreacted MDP2P during workup. A real winner!
Title: What is the "Safest" highest temp for Methanol?
Post by: Bubbleplate on September 18, 2002, 10:10:00 PM
What is the "safest" (i.e., no fire or explosion) highest temperature for Methanol in a MM Reflux? Although SWIM would run it as recipie says: "reflux should be unnervingly vigrous...with MeOH dripping really fast down out of the condenser" he'd still like to monitor the temp. with a thermometer. What's the upper temp?
BTW: The Sassy Oil that went into this dream was from Sassy roots collected by SWIM. From ROOTS TO ROLL! Nature hikes rock - The War Is Over! If they drive God from the earth, we shall shelter Him underground - Dostoevsky
Title: Whatever you do to methanol, it will never get ...
Post by: Rhodium on September 18, 2002, 10:41:00 PM
Whatever you do to methanol, it will never get hotter than 64°C, unless you try to pressurize the container.
However, depending on the addition rate, the methanol can boil more or less vigorously. Just monitor how fast you can add your reactants without flooding the condenser.
Title: Re: Methylamine formate is the reageant Has ...
Post by: El_Zorro on September 19, 2002, 04:13:00 AM
Methylamine formate is the reageant
Has anyone tried to synth N-methylformamide by heating methylammonium formate until water distills over, like with ammonium formate-->formamide?
Who is that masked man?
Title: Why would anyone want to do this?
Post by: terbium on September 19, 2002, 05:19:00 AM
Has anyone tried to synth N-methylformamide by heating methylammonium formate
Or are you trying to ask if anyone has done a Leuckart starting with methylamine and formic acid?
Title: something like that, I was wondering if anyone ...
Post by: El_Zorro on September 20, 2002, 12:07:00 AM
something like that, I was wondering if anyone here does the N-methylformamide leukart, and if anyone wanted to do it but they couldn't get the N-methylformamide, would it be possible to synth N-methylformamide by dehydrating methylammonium formate by heating it, just like the ammonium formate-->formamide synth. Who is that masked man?
Title: Leuckart
Post by: terbium on September 20, 2002, 05:19:00 AM
Yes, you can do a Leuckart using methylamine and formic acid as starting materials. It is not necessary to isolate pure n-methylformamide, you just mix the aqueous methylamine and formic acid in the flask where you are going to do the Leuckart and distill off most of the water before adding the ketone.
The Leuckart, though, seems to give much better yields for amphetamines than n-methylamphetamines. Also, I have only done the Leuckart with plain P2P, I wonder about the stability of the methylenedioxy ring under these reaction conditions with MDP2P.
If you use the search engine here and search for "Leuckart" you will get a couple hundred hits.
Title: Oh shit, the old man's tellin' war stories!
Post by: El_Zorro on September 20, 2002, 11:27:00 PM
I gotta tell you, terb, I do love hearing your stories of the good old days of clandestine chem. You should write a fuckin' book or something. I know I'd buy it. Or at least a post on the couch.
But as for the leaukart, I don't really think I'll be doing the leaukart anytime soon. It seems like it would produce too many byproducts. Nothing vac distilling the freebase wouldn't cure, but still, the only real interest I have in it is doing the N-methylformamide purely for the knowledge that I used one of the most tightly controlled chems around, and in a way not normally done. Who is that masked man?
Title: WTF!?!
Post by: tranceport on September 22, 2002, 07:22:00 AM
Title: :redundant
Post by: hellman on October 10, 2002, 09:05:00 AM
No offense ROUNDBOTTOM, he will be doing 1kg amounts,-as you are,
don't make this any harder than it has to be,. don't psyche the guy out, we all now how easy it REALLY IS!!, if you plan and are motivated, whooooaah-[the count style'] I appreciate your iNput, and acknowledge your wealth as a human, but you are you, and he is he, why would you think for a second that he approaches events similar to you,
-i heard it all before, yeh.... so, it is a highly guarded and tech. industry,.which, sigh , tends to breed arogancy,-(in the nicest possible way of course) but perpetutating this is going against the grain of what we, here at the hive are about,.
-It would seem that I could be susceptible to diminishing my karma points, so it would seem, woh woh woh whooooaa
big smile, love you all, don't bite the hand that feeds you, comprende.......
SHARE :) IQ is the rate of logic, as Wisdom increases logic, fear & compromise decrease to reveal objectivity
Title: Mad Props to Bubbleplate!
Post by: No1CockSucker on October 14, 2002, 01:41:00 AM
Now you are almost 1/2 way there. I would do the MM Al/Hg from there if I were you.
And then (and this is the best part), next time you can dispense with the safrole and cook up some elemicin & some myristicin.
YES!!!
HNT: The LEUCKART will come in handy in those instances I believe. It's super klean and EZ if you watch the temperature carefully.
Title: glad to help!
Post by: wyndowlicker on October 14, 2002, 03:58:00 AM
Congrads bee!Your well on your way!MM al/hg+nirto is beautiful.use it,live it,eat it. :P You can tell the queen of diamonds,by the way that she shines.-GD