07-01-03 08:43
No 443689
Raf was wondering if 30 liter PolyPropylene bucket could be used in performic acid oxidation.DCM doesn't readily dissolve PP afaik,dunno about isosafrole,but iso isn't in pure state in reacton but dissolved in DCM.Also whole mix is an emulsion cuz it's stirred hard during rx.Comments are welcome
For those about to synth,we salute you
(Hive Addict)
07-01-03 09:11
No 443702
Raff, If you are looking to upscale I suggest you check out Labtops Large reaction posts on the "buffered Performic". If you are not very careful you can end up with a dangerous exothermic reaction. I would not want to do that in a PP bucket.
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(Hive Addict)
07-01-03 10:09
No 443721
Yeah,i've read em many times.He says to use SS but PP should work also.Rx temp can't rise over 40C(reflux) anyway and raf plans to use his 3 feet Aldrich super condenser in this dream.Labtop's writeup calls for 120 kgs which is bit too much for SwiRaf's friends.
Post hydrolysis ketone matrix will be distilled in small amounts(like 100 grams at the time,rest waits in the freezer) to prevent excessive polymerization
For those about to synth,we salute you
(Hive Addict)
07-01-03 11:07
No 443736
i've said it before, i'll say it again. pyrex carboys are the ticket. anywhere from 9L up to 36L. made of borosilicate. heavy wallled. fit a #12 stopper in the spout. have a beer making supply place drill a hole 24mm wide (the 24 in 24/40). then you can place a claissen in the stopper and affix all sorts of goodies like overhead stirring, addition funnels, and condensers. if you find one that is aspirated, voila! 20L sep funnel.
performics of admirable size are simple... use standard glassware for the distillation. multi-kilo size MeAm reactions, same as above. fair sized Al/Hg Amalgams with foil and MeNO2 if you're still into that.
two ways i can think of to heat them, should you need it. get a large institution size pot that will fit the carboy and fill it with hot water of the desired temperature. alternatively, get a heating tape. like a heating mantle, but in a flexable, sometimes rubber coated, long ribbon. wrap it around the carboy as many times as possible, then connect to your mantle controller.
these ARE NOT, repeat, ARE NOT beer and wine making carboys. same idea, different material.
Now with 12% more Bottom!
Nymphomania is not a disease, its a goal! (Methadist)
(Hive Addict)
07-01-03 12:23
No 443745
Heating isn't needed.Vessel is only for performic acid oxidation.Even wine carboys can temp 40C with no problems.For isomerizing a la LaBTop,SS will be used.
230C and 3 hours.Reflux isn't needed AFAIK and 230 C will kick water out w/o problems.For 15% H2SO4 hydrolysis,SS reactor will be used.80 C and 3 hours as usual.Distillation of post-hydrolysis ketone matrix will be very time consuming,especially if pump is weak and brings ketone over at 140-150C - one must distill in small batches.
For those about to synth,we salute you
(Hive Addict)
07-02-03 08:37
No 443919
I have thought about a SS rig also Raff, but I figured that the H2SO4 Would mess with it or play with the reaction.
I eat "Bad Karma" for breakfast
(Hive Addict)
07-02-03 08:53
No 443922
15%H2SO4 is pretty violent stuff,i guess it depends on what SS one uses.Some SS's are called acid proof or "inoxidable" or something,they make pool ladders out of em,maybe these could handle it.One also needs a thermostat which can keep mix around 80C,using variac is not recommended:it's difficult to stabilize temp with it.
For those about to synth,we salute you
(Hive Addict)
07-02-03 08:57
No 443923
absolutely, yes!!!! DO NOT use SS for the H2SO4. SWIM tried that in a 10L SS pot, temp got a bit too high (like 90C-95C) and the whole reaction turned a dark copper green, and completely useless. nothing recoverable. and it wasn't a cheap SS pot, either. SWIM has no experience with H2SO4 and PP or any other plastic.
Now with 12% more Bottom!
Nymphomania is not a disease, its a goal! (Methadist)
(Hive Addict)
07-02-03 09:03
No 443924
I was diluting some H2SO4 on the kitchen sink when I accidently knocked over the bottle. The sink top had permanent discoloring as a result, even though it was washed down immediately.
Interestingly, Labtop talks of using SS equipment in his sooperdooper big Performics.
I eat "Bad Karma" for breakfast
(Hive Addict)
07-02-03 09:04
No 443925
my bad...must find some big flask,he has a 12 liter one,but how he should attach rheostat?He can't just dump some probe into rx mix,can't he?
For those about to synth,we salute you
(Hive Addict)
07-02-03 09:05
No 443926
Interestingly, Labtop talks of using SS equipment in his sooperdooper big Performics.
Yeah,that made me wonder,i don't think LT is talking out of his ass,his atmospheric safrole isomerization worked like charm.
For those about to synth,we salute you
(Hive Addict)
07-02-03 09:07
No 443927
Raff, the temp. doesn't have to be exactly precise. Why not just stabilise a water bath at 85. C?
Or, use methanol to keep the temp. in check?
I eat "Bad Karma" for breakfast
(Hive Addict)
07-02-03 09:16
No 443929
In raf's experience,80-85 C is best temp for hydrolysis.2 hours seem to leave some glycol unhydrolysed,3 hours seem to work just fine.Methanol is just like asking for trouble,if mix starts to reflux,one also needs to use a condenser which renders overhead stirring difficult.If using water bath,thermostat is still needed.Raf is sure there is some way to easily keep that temp stable.
For those about to synth,we salute you
(Chief Bee)
07-14-03 00:36
No 446910
Different stainless steels handle acids differently, they are not a single alloy. LT obviously refers to an acid-proof SS variety.
(Newbee)
07-14-03 03:52
No 446940
Swim has a 2 litre PP container with overhead stirring and condensor attached. It sits in the top of a stainless steel water heater making a water jacket that can be heated to 104 -110 celcius (if salt water is inside) or can be flushed with cold water at will to bring it to 0 celsius. Very easy to control all temperatures in the below mentioned reactions with this system!!. Swim has used it many times for:
Modified performic- dcm or chloroform
H2SO4 perfromic hydrolysis
Al/Hg amination with MeAm.HCL
to make MeAM.HCL via different methods involving Ammonia, HCL, Formalin, formic acid and temps 104+ celcius.
The PP is not affected in any way nor is the product.
"Now they call taking drugs an epidemic - that's 'cos white folks are doing it - Richard Pryor.
(Hive Addict)
07-16-03 12:52
No 447757
(Rated as: excellent)
This works like charm,no problems doing 0,5 kg reactions.Overhead stirring and external cooling as you can see.Inside the PP cooling jacket there is 7 liter 3-neck roundbottom.Stirrer is made out of power drill and variac.Works for hydrolysis also.
Performic reactor
400 grams of isosafrole being oxidised
Hydrolysis of glycol in 3 liter 3-neck(from 400 grams of isosafrole) with 2,4 liters of 15% acid
Same setup
For those about to synth,we salute you
(Hive Addict)
07-20-03 21:30
No 448683
If needed,raf will post more pictures.From that 400 grams of iso(iso was good,d20 1.120 and even bit more,safrole had a d20 of 1.095) he ended up with 245 grams of ketone,could have been higher but he has a lousy vacuum pump and some ketone scorched.Ketone seemed good,he aminated 60 grams at the time and constantly got 44-46 grams of amine hydrochloride out of every 60 grams of ketone(he did four runs).
For those about to synth,we salute you