Francis_7 (Stranger)
06-27-02 09:01
No 325962
      RoundBottom, greeter, where are your BA results?  Bookmark   

Where are the results to your bucket amination trials?  (Yieldwise.)

For awhile there, both of you were on a roll and then suddenly--poof!--you were gone!

For newbees, I gotta tell you, leaving us hanging there--like you have been doing for about a week or two--it's just fucking mean.

(Hive Addict)
06-27-02 10:37
No 325988
      wrong dude.  Bookmark   

i think you're looking for FlatBottom.  RB never had anything to do with a bucket. 

i learned a thing or two from charlie dontcha know.
(Hive Bee)
07-01-02 15:14
No 327566
      bucket results  Bookmark   

Thought I had posted this information, but ok...

An anonymous letter I received reported results from two MM Al/Hg aminations, one at 'normal' (25g ketone) scale in a 2L flask and one at 4x (100g ketone) scale in a bucket.  After working up the 25g run (see another post for the gory details), the chemist had some dirty mdma freebase in DCM (although, as stated before, based on most people's standards this would have been considered very clean--yuck).

The letter goes on to say that the chemist judged this amount of mdma freebase insufficient for distillation in the available glassware, so more freebase was sought...  thus the 4x scale MM in the bucket.  The bucket lid was built pretty much as described in the pics on Rhodium's page, although the chemist reports that finding a shank washer was difficult until he looked specifically in the hardware store's section for replacement toilet parts.  Also, the chemist punched another hole in the bucket so the addition funnel could sit in the lid rather than the top of the column.  This turned out to be a VERY good idea as the reaction go so hot it literally burped out methanol from time-to-time (burped out of a 40cm condenser sitting on 60cm of vigreux column!).

Based on advice given HERE, the chemist apparently went ahead and tried to stir this reaction with a 3" stirbar on a magnetic stirrer.  This was a total failure.  DO NOT try and stir this reaction at this size with magnetic stirring.  The stirbar just got stuck early on and then there was this pissed off hot reaction to contend with.  Not cool.  This reaction needs overhead stirring at this scale.  The chemist feels his yields were shit because of the lack of stirring.  Furthermore, at this scale, this is an ungodly amount of solvent used, waste produced, etc.,.  The chemist reports that he will probably *never* run the Al/Hg with nitromethane again ("fuck that", he writes).  The workup is just too much of a pain in the ass.

For future runs the chemist has apparently decided to go with Osmium's methylamine Al/Hg.

As far as the low-down dirty details:

The freebase in DCM from the 25g rxn was combined with the freebase in DCM from the 4X 100g reaction, and the lot was then distilled.  The chemist recovered 81.5g clean mdma freebase oil, or a 60% molar yield.  He thinks had overhead stirring been present the yield would have been much better, but it still would have been a massive pain in the ass to work up (remember, you gotta RECOVER all that toluene and dcm for reuse later).

A watched pot will indeed boil.
(Hive Bee)
07-01-02 16:15
No 327575
      Question..  Bookmark   

Did the chemist add the nitro before the ketone, or simultaneously?
all three reactions produce heat.
(Hive Addict)
07-02-02 03:49
No 327817
      For best results  Bookmark   

For best results add the  nitro before the ketone.  The nitro usually reacts very quickly and this part of the rxn produces the most heat. The response time of heat to the addition rate is very fast. It is pretty easy to judge the progress of the rxn. if the foil is balled up into tiny balls it is much easier to stirr. If your still having problems then go spen 1.99 on a liter of Ipa at the supermarket and add it to the rxn if stirring becomes difficult.  Better yet shop around and find a ultra beast stirrer 9000 and a 4 or 5 inch bar.if your burning 80grams of shit at a time then surly you can afford something better than what you got.  Also the ketone can be added pretty quickly This part does not produce that much heat.Pay attention to what your doing and everything will stay in the condensor.  If you have a pressurized funnel the use a clasien and puta condom on the top.  this is advantqageous any ways cause with a closed system more of the MeAm formed stays in solution to react with  the ketone as soon as it's entered into the system.  A better plan than using nitro methane is to make a ton of Me Am before hand in the bucket the n Use Me am crystals with some sheet alumnium.  Imagine how much tone could be burned with sheet in a bucket??<>?<><
Muhahahah  wink
(Hive Bee)
07-02-02 05:22
No 327841
      simultaneously  Bookmark   

The nitro was mixed with the ketone in the addition funnel, per MM's instructions.  It was just a 4x scaleup, except that instead of using 1600mg HgCl2, 1g was used which was plenty.  800mg would have probably been just fine too.

As far as heat, yes they all produce heat, but as I understand it the seriously exothermic rxn is the conversion of nitromethane to methylamine.  The bucket is a good place to run the reaction, just not with a normal size (5"x7") hotplate/stirrer.  Future runs will involve the bucket, MeAm.HCl, and overhead stirring.  Then all will be well in the universe.

VL:  Adding more IPA/methanol won't do a damn thing to help a 3" stirbar get going.  It was tried!!  The problem is as the foil breaks down the sludge builds up on the bottom of the container and just creates too much resistance for the poor stirrer to overcome.  At 4x scale you either need overhead mechanical stirring or yes the Ultra-Blaster Magnetron 9000(tm) that MaDMAx has.

Just don't get your nuts too close to that one...

A watched pot will indeed boil.
(Hive Addict)
07-02-02 06:59
No 327863
      stirrers  Bookmark   

If you run a bucket you can afford a nice stirrer. don't be cheap.
(Hive Bee)
07-02-02 11:36
No 327946
      stir rod  Bookmark   

how would you seal the stir rod on an overhead stirrer, a lubricated o-ring maybe.
By seal, I mean prevent gas leakage from the opening where the stir rod enters the system.
(Hive Bee)
07-02-02 16:44
No 327999
      Mercury seal  Bookmark   

The classic method of sealing an overhead stirrer is a mercury seal.  Other high viscosity substances could be used but would require greater depth for the the same results.
(Hive Bee)
07-03-02 01:59
No 328135
      I've seen mercury seals in chem catalogs  Bookmark   

I never uderstood thier general priciple though.
(Hive Addict)
07-03-02 04:20
No 328179
      long shaft  Bookmark   

Well, if you have a long shaft (cough), you could run it down the condenser easily. You will have to feed it through the condenser from the bottom obviously, then assemble it all together.

there's a big difference between criticizing your government and criticizing your country
(Title on BackOrder)
07-03-02 04:32
No 328184
      sounds like an accident waiting to happen  Bookmark   

All that long rod has to do is catch on a chunk of aluminum and you might have a mess on your hands.  Just use a multiple necked flask and stir through one of the side necks.

All paths are the same: they lead nowhere
(Hive Addict)
07-03-02 05:29
No 328199
      opposite  Bookmark   

put the condenser on a side neck, and the stirrer on the centre.  that's why 45/50 necks are in the middle, so you can get large propellers in.

i learned a thing or two from charlie dontcha know.
(Hive Bee)
07-03-02 06:32
No 328214
      Thanks  Bookmark   

That's good advise, I seen those setups before just forgot about 'em.