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Author	Topic: Ketone for lazy people
KrZ Member	posted 01-12-99 01:32 PM I'll have to admit I'm pretty slak when it comes to shaking a coke bottle so recently the R&D team here has developed this vessel which has yet to be fully tested. The stuff we used; 1 ft long 10" diam piece of PVC pipe 2 end caps for PVC pipe 2 x 1/2" male-male brass connector Tire valve 1/2" brass screw-on endcap PVC pipe sealer 2 nuts to attach to the male-male connectors Gasolia Soft-Set Thread Sealant with Teflon Tire Pressure Gauge Tank of Welding O2 1/2" Hi-pressure hose with screw caps (3ft or so) Elec. tape or whatever 4l beaker, stirbar, stirplate Take the PVC end-cap and drill 2 1/2" holes and one hole big enough for the tire valve. Put some Gasolia on the male-male connectors and screw them into the 1/2" hole. Screw the nuts onto the connectors on the inside of the PVC caps. install the tire valve and use some gasket sealer to make sure its nice and tight. Seal the untouched PVC endcap to the pipe with the PVC compound. Place the capped pipe on the stirplate. Slide the beaker inside of the pipe (if its loose put some paper towels in there to stablize it and don't make it a tight squeeze so its hard to get out either). Place your standard list of SRV reactants in the beaker. Drop the stirbar in. Smear the Gasolia on the inside of the other PVC cap. Place the cap on the pipe and pull up and down while twisting so you ensure a good wide seal between the cap and pipe. Make a full loop with the tape around the hole pipe just do be sure (I did it twice to make an X pattern on top/bottom). Screw the hose onto the tank and brass fitting. Attach the tire pressure valve (If you've got a regulator on your O2 tank this isn't necess.). Spray the O2 into it with the other connector open, this way it pushes the atmosp. out. Cap the other male-male connector using Gasolia. Pressurize it on up to 125 psi (thats as high as I took it but who knows). Turn the stirrer on and wait 2 hours or so... You get the picture... Anyway, the device has been constructed and pressure tested, but no runs yet. I'm assuming you would need to give it 2 hours but it could be less considering the ridiculous amount of O2 we'll be cramming in there. Its certainly alot harder to make than an SRV but once you've got it setup I think it has some minor advantages, I'll provide an update on how it goes in action as soon as I can.
Bright Star Member	posted 01-12-99 03:00 PM Go Boy!
Orpheus Member	posted 01-12-99 03:04 PM KZR: that sounds like a good idea.. the only problem i can see is wether or not magstirring can give enough agitation.. It would be nice to hear of any dreams of this being tested... Orph
ChemHack Member	posted 01-12-99 05:33 PM If you forgo the beaker and just put the liquid in the PVC will it melt the plastic? What about using that special grey "chem resistant" kind of PVC ? Has anyone ever tried PopEye's SawZall/Skateboard trick with an SRV ?
Orpheus Member	posted 01-12-99 07:55 PM KzR: Nevermind about my last post.. A good vortex could definitly be achieved in a flat bottomed flask.. you could even use a Large pyrex pot if you don't have access to a 4l flask ( like me ) a good addition would be of an acrylic window so you could see the how far along the proccess is .. this could be rEal GOOD. about how much did this dream set up cost?? -Orph-
KrZ Member	posted 01-12-99 10:42 PM I got the pipe from a developer friend, the caps I bought 5$ each I think, fitings 4$, (I didn't use the pressure valve I used the regulator from my N2 tank), the hose was 7$, I think the two sealents came to $22 the gasolia is exp. but its guaranteed up to 10,000 psi so I figured that might be enough ;-).
KrZ Member	posted 01-14-99 11:18 AM I'm going to redistill to make sure; In the beaker went; 3.5 g PdCl2, 45g CuCl, 295 g Safrole, 875 ml DMF. Pressurized it up to 120psi, let it stir with a heavy ass vortex for about 2 hours(so hard a large portion of the bottom of the beaker was exposed and shit was way up on the sides). Extraction as usual. Distilled off the DCM and everything else coming over before 142C, then came a fraction at 148C weighed it at 8.6g, and another one at 152C weighed it at 285g. First fraction was yellowish and had an odor, second fraction had no odor and was yellow-light-greenish with no smell. Remember this vacuum pump is retarded, it pulls safrole over at 127. I also tried using the silicone glass-joint stuff to make a seal and it didn't hold as well as the gasolia (I could hear it leaking). The room it was done in was about 50F.
Beagle Member	posted 01-14-99 11:27 AM ABS (black or grey) plastic tubes would be MUCH preferable to PVC. When failure testing PVC pipe, it is seen that the PVC will shatter into millions of sharp fragments. ABS has a much higher pressure rating, and when it does fail, it will only split, not turn into shrapnel.
KrZ Member	posted 01-14-99 11:47 AM Thanks Beagle, I had a little wooden shield around it because I was scared it would blow my ass to high-heavens! I'll try and find a big-ass pipe of ABS, I'm gonna try and find some pressure ratings too.
Bright Star Member	posted 01-14-99 03:30 PM AMINATE! AMINATE! AMINATE!
Orpheus Member	posted 01-15-99 01:26 PM I was under the impression that the Ketone should smell kinda like cardamon.. maybe i should stop rereading those old Zwitt Docs.. KzR: you say it had no smell?? have dreamed of aminating a small portion ov it to see if it produces honey?? i would be very interested in the results.. PS. Sorry that i'm unable to input more on this.. i don't have lots of lab equip or chemicals.. i'm also short on money and experience.. i'm looking to others for help and any feedback on variations and methods that definitly work and are fairly easy. Sweet Dreams - Orph
TheCat Member	posted 01-15-99 01:34 PM Correct me if I'm wrong (which is a strong possibility) but isn't 285g of ketone from 295g of sassy about an 88% yeild? Have you thought of using a solvent other then DMF, maybe something a little over the counter like IPA? Hey if you used IPA you could toss in some isopropyl nitrite ala drone and get a little more bang for your buck. Just an idea. Peace TheCat
Semtex Enigma Member	posted 01-15-99 02:02 PM KrZ: What is holding the top end cap on? From what I have read it is some kinda soft set and some electrical tape. If the soft set enables you to remove the end cap later on then great, if not how does one open this vessel and remove what one has made? Please tell me you didn't run it up to 125psi with the only thing holding the top on being electrical tape...
quirks Member	posted 01-15-99 02:05 PM The lower tempeture stuff distills at the less it seems to smell.
TheCat Member	posted 01-15-99 03:46 PM KrZ I love your adaption of the SRV. I had another idea. What if you added another preasure regulator to the vessel to let O2 out. What you would get would a constant supply of fresh O2. You could even hook the input side of things to a dispersion tube so that the fresh O2 would be bubbled through the reaction solution and hopefuly increase absorbtion. Just and idea. TheCat P.S. Another note on the solvent, it would be nice to use IPA as the solvent due to the fact that it boils at a much lower temp (about 82 deg C) compared to DMF (b.p. 153 deg C)
KrZ Member	posted 01-15-99 09:37 PM I ended up putting in the tire valve so just push on the needle. If you do plenty of tape lengthwise, it was not a problem, do multiple X patterns thtas what I used, seemed to hold, but it could have been about to explode for all I know, it made me so nervous a stood in front of it and took bong hits jk Pipes can handle good pressure obviously, especially the 10" shit which is really thick, I had to get it at a specialty place cuz they didn't have it at HD. The gasolia SOFT-SET worked to seal it. I was very sloppy w. cleaning, one small oil spill on the bench I probably lost 10ml or so, thats why the 88%. Would have been 90's...
TheCat Member	posted 01-16-99 11:58 PM Hey KrZ, have you had any more high preasure dreams latelly? I would love to hear of the results if you have. I was wondering have you though of trying to increase the preasure to say... 300psi or so. What did you pay for your tank of O2? I have been looking around the web for tanks of O2 and when I was reading the Air Products wep page they say that a standard tank will only deliver 100psi (even though the standard tank is charged to about 1660psi @ 70*F) due to the fact that the regulator has a limiter. Peace TheCat
KrZ Member	posted 01-17-99 10:57 AM I went to a local welding supply place, they had regulators that went up to 100, 125, 150 and various other levels (with increasing cost the higher it was rated for) the one I got goes up to 125, as you might have guessed. It was a pain in the ass finding an adaptor to get it to connect to the 300psi presssure hose I bought, it was a 5/16" size regulator and the hose was 3/8", apparently a very uncommon combination cuz I had to go 5/16->1/2->3/8 with brass adaptors to hook it up. I'm perfectly content at 125, I didn't wash the filter cake when drying, left ml's of oil here and there in beakers, and knocked over a 250ml beaker with some oil in it, so I believe actual yields were very high. The PVC I bought only came in a 10ft piece at a time (got funny looks from the counter guy when I wanted only 1 ft) so I've got a big piece sitting in my backyard. I'm going to get an ABS pipe before I do it again as it seems Beagle was quite right (after reading up on it). Trying to think of a way to fit a big rubber o-ring around the inside of the pipe and designing some latches for quick snap-on loading ;-) I'm pretty satisfied with all yields but, I want to get something real nice and take a pic. of it and upload it for you guys to see. Amination is currently proceding under nitrogen using 300g of MeAm in just enough MeOH to dissolve it (you need to dissolve the MeAm in methanol first and it takes an hour or so of careful checking + addn. to get it perfectly saturated, which is important!). You don't need to waste a kg!! Just wait longer, check the pH and adjust accordingly, use heavy ass stirring and you'll get the same yields!!
TheCat Member	posted 01-20-99 07:30 PM KrZ, did how did the Amination go? Peace TheCat
KrZ Member	posted 01-20-99 09:14 PM You skimp on MeAm and you end up waiting 4 or 5 days, I don't mind, easy enough to have 20 going at once ;-)
TheCat Member	posted 01-20-99 10:16 PM KrZ, one more thing. Have you had anyone more dreams at high preasure? If you have how were the yeilds? Also I was a thinking. You want a nicer looking presure vessel? Go to the plumbing store and ask for a "clean-out" for you 10" ABS or PVC pipe. What a clean-out is is a section of pipe that looks kinda like an end-to-end pipe coupler with a big ass threaded plug in one side (if you go ask for one you will know what I'm talking about). What you would do is put the regular end cap on one end then attach the clean-out to the other end and there you have it. A preasure vessel with a screw on cap. Peace TheCat
KrZ Member	posted 01-22-99 02:12 PM A 2l beaker full of IPA in my freezer is now full of 1mm Snowflakes, I'll be sampling this tonight :-)
TheCat Member	posted 01-22-99 06:35 PM Hey I'm kinda curious about your yeilds from aminating with only 300g of MeAm. How much ketone did you aminate with that? Also you said that you had a 2l beaker full of snowflakes in you freezer, did you crystalize it in that or did you crystalize it in DCM and recrystalize it in IPA or something? Peace and congrats on the bad ass yeild. Does anyone know of any other process that gets yeilds in the upper eightys on a regular basis? TheCat
Semtex Enigma Member	posted 01-22-99 08:59 PM Small correction/note: The purpose of a regulator in situation which you are describing is not correct. You see when a regulator(say 125psi) is hooked up to the O2 tank, all it is doing is regulating the flow of gas through the tube from the regulator at a maximum pressure of 125psi. It does not control the pressure in the vessel, only how fast the gas enters it. To get an accurate reading of the pressure inside the pipe one would have to equip the vessel with a gauge. I once suggested a modified version of Piglet's proposed bubbler for the wacker. You see I think that bubbling under atmospheric pressure would be uneffective, however I have reason to belive that it would indeed work under increased pressure. I will try to write up an outline for those in the position to dream of such things. If anyone is interested please let me know...
TheCat Member	posted 01-22-99 10:17 PM Semtex Enigma, I have been wanting to make such a device for months. Unfortunatlly I have no money and I am going to have to wait months till I could even thing of trying such an idea. Peace TheCat
KrZ Member	posted 01-23-99 12:03 AM It was about 80%, theres still some more rexytal. in the IPA now so I don't know exactly yet. I just waited a little longer, was very careful dissolving my MeAm to assure saturation, and I filled it with nitrogn and capped w. a ballon each time, I also checked and adjusted the pH with a digital meter every 6h. Other than that its all been said before... I told the guy at the welding place I would be injecting N2 into soil for an Ag. Exp. involving ag. engineering; oxygen/nitrogenation injection cost analysis for farms, etc. he believed every word, he said I'd need a tank and regulator, then he produced a brass piece with two pressure gages and another steel piece that fit into it with a big plastic knob and another gag, he said just hook the flow regulator to the tank and the pres. regulator up to it. Thats what you get for welding standard set up right? If the flow reg. was just on there I suppose all 1000osi or whatever that tank is at would come across, boooom! I've been looking at these stainless stell compressed gas tanks MSC direct has, 4.7 gallon capacity one for ex., some welding to attach a mechanical stirrer would be needed for anything bigger but I think a big stirbar and some fine tuning of the plate to get max spin would do it for this size. Could form alot of ketone that way....
TheCat Member	posted 01-27-99 10:12 PM KrZ, I've been contemplating using a five gallon bucket at a presure vessel. Attach the inlet and preasure gauge to the lid just like you did with the pipe, toss in a BigAss Stirbar(tm) and duct tape the fucker closed. The great thing is that most five gallon buckets are high density polyethylene so I figure that there won't be any need for a beaker or flask. Imagine it, you could do ten liters all at once in the damn thing. Now thats alot of ketone. Peace TheCat P.S. Do you have the part number for that tank from MSC?
hellman Member	posted 01-27-99 10:59 PM Would love to see a picture, I'm sure an proceedural account of your amination would charge a few glasses. hellamsnski.
TheCat Member	posted 02-03-99 05:27 PM So has anyone other then KrZ tried this variation of the Wacker?
Bacchus3_4 Member	posted 02-08-99 02:34 AM Krz- If I wouldn't be intruding, I'd like to take a Wack (no pun intended,) at a couple of improvements. May I?? ------------------ Bacchus
KrZ Member	posted 02-08-99 10:00 AM Of course! I'm no engineering specialist by any means so go right ahead all suggestions/ideas welcome.
TheCat Member	posted 02-08-99 03:16 PM In the next few weeks I'm planning on bringing out the old cracker box and welding a presure chamber out of some .25" steel that I have laying around. I'm thinking of using a pump seal so that I can pass a 1000rpm rotating shat through the box for stirring. For about a second I thought of puting the motor on the inside of the box but I figure with a 150psi pure O2 enviroment and a whole bunch of methanol a single spark from that motor would turn the whole thing into a fuking gernade. Peace TheCat
Bacchus3_4 Member	posted 02-08-99 04:58 PM Krz, Will do. I'll post complete details within the next couple of days. Also- Be on the lookout for another post detailing how to make yourself a quality hotplate/magnetic stirrer for under $100 from yours truely. late ------------------ Bacchus
TheCat Member	posted 02-08-99 10:36 PM Bacchus: Just one quick question. What are you planning on using for the heating element? I'm deffinitlly interested in your design, I want to see how it compares to mine. Sorry for being so impatiant. Peace TheCat BTW - If I get the time I'll try to post my design.
Bacchus3_4 Member	posted 02-09-99 03:49 AM Cat- The heating elements from electric stoves generate quite a bit of heat 250-300c (I checked today,) and probably more if they are placed in a properly insulated container. they are also easly hooked up to a variable resister to control the temp. I'll try to post complete details by tomorrow evening. Sweet Dreams ------------------ Bacchus
psychokitty Member	posted 02-09-99 03:57 PM TheCat: Your idea about using a plastic 5 gallon bucket is right on the mark. But wouldn't it be better to buy one a bucket from one those plastic companies that specializes in such products -- one that has a scew-on lid already incorporated into its design? This way, you can get in and out of your reaction vessel without having to remove so much tape or adhesive. KrZ: Your design is stellar. --Psychokitty
TheCat Member	posted 02-09-99 07:19 PM psychokitty, I have also though about using a containder with a screw on lid the only thing I worry about is that there is going to be about 150psi inside the vessel and I really don't want to know what would happen if that lid blew off. I know that duct tape will definitlly withstand the presure.
Bacchus3_4 Member	posted 02-12-99 06:56 PM OK, As I pormissed earler on- later on today I will post my thoughts on this improved KRV. Also, I will post my complete write up on how to make your own hotplate/magnetic stirrer. late ------------------ Bacchus
Snidely Whiplash Member	posted 02-12-99 11:37 PM KrZ, plz drop me an email when you get a chance. snidely@dqc.org ... Thanks!
Semtex Enigma Member	posted 02-19-99 09:27 PM Krz: Have you done a bio-assay, and if so how was it?
dpHarma Member	posted 02-21-99 01:53 PM Has anyone determined if the wacker will run in a stainless steel vessel? If the steel is not a problem, one of those canisters from pepsi(tm) coke(tm) for soda fountain use would be ideal (I have one ;-)) they have a large removeable lid and two threaded ports, one w/ a tube extending to thge bottom of the canister, the other a short (2") tube. the canister comes eqipped w/ 'quick connect' devices which may be industry exclusive, no luck in matching thread so far. The bottom of the canister is coated w/ hard rubber, which can be burned off outdoors w/ a chisel and propane torch, shoulc one want to apply heat. The device is designed for pressures around 60psi. I've not tested for overpressure. one could fashion a 'beaker' from a 3L pop bottle by cutting off the tapered portion. the bottle bottom and sides could possibly be squeezed through the 'oval' opening to provide a plastic 'liner' of sorts. tinker, tinjer, tinker dpHarma
Semtex Enigma Member	posted 02-21-99 02:42 PM That should work great, except i'd find something flatbottomed to use as a liner, since the stiples in the bottom of the bottle will make mag stirring very uneffective. You should be able to get a pressure rating some where on the container, if not call up Pepsi and ask, they gave out the rating of the 2l bottle to us...
psychokitty Member	posted 02-22-99 08:58 AM As for KrZ's set-up, I have a little bit of information to offer. I spoke recently to a machinist who know something about pressurized canisters and he told me that PVC pipe fittings are pretty resistant to corrosion and could possibly hold up to using the reactants directly in the container itself. But since one can't be sure, it probably would be best to conduct solvent tests. The pressure and temperature ratings of PVC can be found printed on the sides of the pipe so that should make it easier to determine how much of a beating it can stand. I also asked about the danger of explosion and he said that more than likely, there would be no danger as long as the temperature and pressure of the reaction did not exceed the limitations of the pipe's design. HOWEVER, if the pipe was dropped -- not even from very high up -- it could very likely break causing the undesired aforementioned explosion. And BTW, it doesn't matter if it is ABS or PVC or whatever as the impact from the released air alone could cause serious injury. As for the easy access issue, the ends of the piping could be threaded, or installed with a threading adapter. KrZ: I must admit that I am confused as to why you use so much O2 pressure when you could easily get away with less. We all know that 30 pounds is effective at transforming the alkene to the ketone in alcohol solvent in 2 hours using just regular air! So why not simply start with a little over 30 pounds and once the oxygen gets used up and the pressure goes down (to just a little under thirty pounds), simply inject more oxygen until 30 pounds is reached again? Just a thought. --Psychokitty
KrZ Member	posted 02-22-99 11:35 AM You're right. I must have had some kind of fucking death wish taking it up that high. I just wanted to see how insane my little creation could get, but it was probably pretty dangerous. I'm not noted for safety, me and my best friend in high school blew-up a deserted grain silo out in the woods one summer, nearly got killed by that shit, a huge chunk just missed us.
Semtex Enigma Member	posted 02-22-99 02:43 PM Psychokitty: It's not the ABS/PVC which I would be worried about melting either, it would be if the solvent disolved the cement/glue which is holding it together thats what I would be weary of. Krz: Was bio-assay preformed? If so, how was it???
KrZ Member	posted 02-22-99 07:45 PM It was good.
psychokitty Member	posted 02-22-99 07:51 PM That's the purpose of threading your pipe so that there is no need of any glue. --Psychokitty
dpHarma Member	posted 02-22-99 08:24 PM the pipe of choice is HDPE high density polyethylene. a great deal of study has gone into plastic pipes used for launching pyrotechnic aerial shells. when a shell explodes in it's launching 'mortar', the total combustible material is comsumed at once (or nearly) and the forces are confined in the tube. PVC and ABS shatter into many small sharp fragments. HDPE tends to deform first and producess much less shrapnel. dpHarma
psychokitty Member	posted 02-22-99 08:35 PM Cool. So where does one get some? --Psychokitty
equarius Member	posted 03-20-99 03:58 PM KrZ; could you confirm your ratios of 45g CuCl to 3.5g PdCl2. Why did you use so much CuCl? You did the amalgamation under Nitrogen, under pressure and a closed system? Used the same reaction vehicle?

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