05-20-02 22:13
No 311702
Cheeser just recently manufactured a small amount of 1-(1,3 Benzodioxol-5-yl)propen-2-none using buffered Potassium Monopersulphate on 2-Alkene to desired Epoxide then further rearranged to Ketone using 15% H2SO4 reflux for 2.5 hours. The ketone was washed with basic washes but was not able to be distilled using vacuum. The ketone tested positive when a big as bunch of chicken fat like solids formed in metabisulphite test vile. there was so much fat chunks in there from just 4 drops of light brown ketone, cheese thought that it would be OK to aminate as is. Using sodium cyano and ammonium acetate. cheese tried but failed at aminating the phenylacetone. Does anyone know why the crude ketone failed in reduction? Cheese thought it would be OK as it passed the bisulphite test with flying colors, big yellow chunks of fat in less than 10 minutes of shaking in metabisulphit solution. Almost there, back to the 'ol drawing board. OXONE ROX!!
<Cheeseboy-a whiteboy with soul, like a black guy without soul
May De Sorce Bee Wit Chu-Always
(Chief Bee)
05-21-02 03:54
No 311798
The impurities may play a role, as you surely understand.
You have not said anything about how the amination was performed, so we cannot help you further.
(Hive Addict)
05-21-02 11:37
No 311997
Post 311995 (Vibrating_Lights: "Amine jewlrey", Methods Discourse)
(I'm not Cheesie)
05-21-02 13:46
No 312084
Thanks VL but cheese's pump is weak ass. Rhodium: The amination was done in a 500ml long neck flat bottom with a GGstopper. Using the above mentioned reagents. No MDA. Maybe the ketone wasn't dried or else the impurities did get in the way eh. Who knows? Trying again.
<Cheeseboy-a whiteboy with soul, like a black guy without soul
May De Sorce Bee Wit Chu-Always
(Chief Bee)
05-21-02 13:54
No 312088
As you know, aminations with ammonium acetate are always very low yielding, even with pure reagents. If your goal is MDA, I suggest you make the oxime with hydroxylamine instead, and reduce that with acidic Al/Hg according to Antibody's writeup on my page. The yields are much better.
(Hive Addict)
05-22-02 03:15
No 312413
Your ketone is impure! High quality ketone will react with bisulfite to form white crystalline shards of the bisulfite adduct. It won't look like chicken fat.
Distill!
(I'm not Cheesie)
05-22-02 12:36
No 312555
Thanks guys. Cheese formed bisulphite sdduct 2wice using metabisulphite. The first time a dark brown slimy cookie formed so cheese took that and oiled it out with HCl 10%, then cheese took that still brown oil and formed another adduct with more bisulphite. The cookie was a little lighter brown but not much, so cheese isolated cookie again and oiled it out to become still a brown oil (dark brown) which does not freeze but is too dark to be pure , by far. Cheese is cared to try distilling it cause the pump cheese has vac distills his isosafrol at 180°C. This would make MDP-2-P's BP at around 220°C-230°C, right? That;s too high right> Someone was saying that MDP-2-P made from the oxone route can be distilled at ATM dude to it's very clean nature of rxn? is that true?
<Cheeseboy-a whiteboy with soul, like a black guy without soul
May De Sorce Bee Wit Chu-Always
(Chief Bee)
05-22-02 12:54
No 312560
According to the literature, yes. I would very much like someone to compare the yields of such a distillation to vacuum distillation though. Something is fishy in my opinion.
What kind of a shitty pump do you use to pull isosafrole over at 180°C? Even an aspirator performs better than that.
(Stoni's sexual toy)
05-22-02 13:30
No 312576
It's not enough to simply form the bisulfite compound, you also have to remove the impurities since they aren't soluble in water! So wash that bisulfite with EtOH and Et2O before decomposing it.
I'm not fat just horizontally disproportionate.