hey matey it would help if we knew what kinds of yeilds you got to answer that one!  If they were 20% probably..if they were 75%+ probably not!

If you could you provide more information it would make it easier to answer and your chances of geting one will be higher

 Things like how much ketone you started with, amounts of solvent and such will help a lot!

What is the best way to get a slow rate reaction?

that depends on a few things but keeping a close eye on the speed of your ketone addition (slow maybe 1 drop per second) and the overall rxn temperature will help by keeping things cool by adding ice to the water bath you (I hope) have the flask in while you are doing the addition

does anyone have any good tips on getting stuck ground glass joints apart    and maybe how to keep them that way?

 My sep funnel has a ground glass stopcock which if left unused for too long jams up.

I don't think it's due to being dirty ... I've been able to loosen it before with heat soap and lots of hassles but now it feels like I'm gonna break it 

 I should really just buy another one but that's always easier said than done

help ideas anyone

Use a heat gun around the stuck joint. Heat around the female joint and with gently twisting of the male joint to loosen. Always grease with vacuum grease.

Ok.
Exampling, some times 5g P2NP in 100ml hot IPA, 150ml Acetic Acid 70% with 7gr Al foil 0,05g HgCl2. First ammalgamed Al foil and wash it and then put in AA70% and IPA P2NP alltogeter. Wait untill reaction go down and reflux a little for 45min. Yiled was 2,5-3grams Dry Amphetamine Sulfate. (sorry i don´t know the propper way to calculate the real %Yield because I very newbee and don´t know too much about kinetic on reactions, I hope learn a lot in this community ).
Another Example, 10g P2NP in 200ml Hot IPA, 300ml Acetic Acid 70% with 12gr Al Foil. Alltogeter in the 1l RBF in water bath and reaction is started with the addition of the solution of small amounth GAA with 100mg HgCl2. yield 5gr Dry AmpSulf.
The last try scalling it up is in a big bottle 3,5L with a Homemade adapter (Pot lid to 29/32), With 100 grams P2NP in 200ml IPA. 300ml Acetic Acid 70% and 140gr Al. All in the bottle and the bottle in the fumes hood in a waterbath (room temperature). Then reaction is started with small amonth of mercury salt in GAA and start to going down a multiples times untiil all Al foil is reacted. The amounth of mercury is just the necesary. During the reaction GAA was added to the botle until the level at all Foil was covered. After basified and extracted two times with refluxing haxane yield was about 45gr dry AmpSulf.

All times the yields was ussually the same (about half of the amounth of P2NP starting on the flask or bottle.) I know it´s not bad beacause yields making P2NP are really high and cheap, but i read people getting about X2 yields than the cat of my dreams.
May bee add P2NP with more IPA to no cristalizate on the adition funel dropwise the reaction would be a good idea.
Any other has a new suggest about the workup.
Thanks!!!
It´s starting to think to run another  step, to make P2NP=>P2P like Fe reduction or tin chloride, and then reduct it with Formamide and Formic Acid. just to make more esay and safe the scale up.
Any suggest to bost yields in Amalgam or recomendation on P2NP=>P2P reaction will be apreciatte.
Oh Sorry! One more question. In the reduction P2P=>Amp with formamide and Formic Acid , Just 85% formic Acid is avaliable. How will that affect the last reaction???
Thanks for your attention and comment.

does anyone have any good tips on getting stuck ground glass joints apart    and maybe how to keep them that way?

Don't store the stopcock in the funnel - some of ours have wire holders although they are annoying - I'm just waiting to hear the sucker go CLUNK against the top of the funnel one of these days.

I got one really good and stuck recently and heating it didn't work.  Spraying it with brakekleen did.  My husband regularly replaces the ground glass toppers with corks when I'm doing several day long separations to prevent it from sticking.

If it is an issue of the stopper being too big or having issues you can regrind it using very fine powders and stopcock grease.  I think I wrote up my husband's procedure for that somewhere's.

 Hi all, i will try to force a lucid dream on iodosafrole route but some questions about the last step are no clear for me.
I read about gassing  MeNH2 in very cold IPA until 15%.
But i found in my "copy and paste archives from the hive" the next answer.
. ON the methylamine HCL question, yes you can but better to put it in some methanol, then add NaOH slowly, the HCL will go off as a salt in the bottom and you will have methanolic methylamine solution, you will get a lot of salt so use big flask
MeNH2 HCl + NaOH => MeNH2+ NaCl +H2O
It's a easy way no doubt about it, But the water formed would be a problem during the reduction.
My question is if the Sodium Chloride amount would be enough to sucks off the water from alcohol keeping the reagent dry to run it successfully. Or if  would be necessary dry it over calcium chloride.
And other question is about running it to MDA, Just substituting MeNH2 for Hexamine. Will run the reaction at room temperature as fast as methylamine?
I know the answers may be on the forum but it's a tough fight for me to find concrete answers using searcher.
I'm  feeling than I'm later.

Thanks Lugh, I hope more luck the next time with the search engine. 

and 4SO you need to do your searches here from the "main" page, the first/front page you see after you log in.

If you try from any other page, like in one of the topics, it wont work properly or more likely wont work at all..took me ages to figure this out!

thanx lugh...I think he's UTSE but getting 'lost' so I'm sure your links will be appreciated

Hi comunity, a new short question about "keto-oxime"was around me the last night.
Reducing P2NP to the oxime what  kind of substance must be found? Is the oxime a solid crystal or is an oil???
Any references about the properties of P2P-oxime would be much apprecite.
I'm lost looking for something about this intermediate...
Thanks!!!.



Special thanks reckless

ones botanic skills are even worse than ones chemistry skills so......

One saw that Vesp asked this about 2 years ago with no answer so ill try again.
Is there any more members of the juniper family that holds safrole then the virginiana?

And about the virginiana, there seems to exist more then one subspecies. Is there safrole in all of them, the one found is called Juniper Virginiana grey owl.
And oh yes one has checked TSE both here and on the www, even looked at rhodiums safrolefaq.

+ isn't it ironic that on this site one gets so many stupid suggestions on the word safrole when one spell checks.....

Thank you....

Hi Carl the amalgam is running safe now.
In the gasoline bucket the best is not try to condense the vapour with any glass condenser. the best safe way is the reaction bucket inside another bucket a little bit more big full of cold water. All the surface will be a condenser!!!.
Then keep the hole open, just covered with a wet towell trying to keep the more amount of solvents inside the bucket.
70 gr of nitropropene are aminated in good yields with no worries about explosion or volcano eruptions.
just amalgam with the minimum amount of mercury salt and if necessary add a Little more when the volcano reaction is going down.
 
P.D: I think than maybee untill 100gr P2NP would be reduce safe in this way

Im glad to know you got it running well 
Oh yes to your new question this is possible of course and is even was the first important route to synthetic vanillin AFAIK, from the oxidation of isoeugenol.
So the general procedure is simply to isomerize your allylbenzene into its propenylisomer, then oxidation of your obtainend propenyl, to the corresponding benzaldehyde.
Bee aware that over-oxidation is very likely to happen and you end up with some stuff like 2,4,5-trimethoxybenzoic acid
here are some useful references from rhodiums archive:
hxxp://www.erowid.org/archive/rhodium/chemistry/isomerizafrole.html
hxxp://www.erowid.org/archive/rhodium/chemistry/piperonal.isosafrole.html