Yep yep yep.. Drengen med for meget fritid gjorde det igen. Sidste gang var det en MDMA syntese, nu er det en meskalin syntese.
Hvad bliver det næste ?
Original:
10 g of Reynold's Heavy duty aluminum foil were torn up and ground up and placed in a 1 liter, 3 neck, RBF. 300 ml of MeOH with a pinch of mercuric thiocyanate were added [Any mercuric salt can be used] and stirring was commenced.
Into an addition funnel was placed 10 g of yummy yellow MDP-2-P, 10 ml of nitroethane which was purchased from a performance fuel shop, yes, I said nitroethane was found OTC, and it really is nitroethane with a boiling point of 114°C, with no engine oil or any crap in it, and a gallon was only a little over $30, and 30 ml methanol.
Once amalgamation had taken place, the ketone/EtNO2 was started dripping at about 2 drips per second until the reaction was going violently. Then drip speed was controlled to keep the reaction going violently, but not out of control. About 15 min were required for the addition. Heat was applied to maintain a reflux while dinner was eaten. About an hour and a half later, the flask was allowed to cool to room temp and 300 ml of 35% NaOH that had been chilled to close to 0°C was added. Then the dark grey/almost black solution was extracted 4 times with toluene.
The toluene extractions were combined, washed 4 times with water and once with brine. A few chunks of baked epsom salts were added to the toluene and it was put in the freezer for awhile. The dreaded HCl gassing apparatus was assembled, the toluene decanted from the epsom salts, and bubbled with dry HCl gas. Precipitate was filtered and toluene gassed some more and more precipitate was filtered, then toluene was gassed again and there was no more precipitate. Precipitate was washed with ice cold anhydrous acetone and air dried. Weight was 8.8 g.
Recrystallization was attempted with 63 ml of acetonitrile, which would have worked beautifully with MDMA, but almost none of the MDEA would dissolve even when boiling. another 63 ml was added and brought to boiling, but still most of the powder remained undissolved. Acetonitrile was cooled and MDEA filtered. Acetonitrile was rotovapped leaving behind a residue of MDEA in the flask. Recrystallization was attempted again with isopropyl alcohol. 350 ml of boiling IPA still hadn't dissolved all of the MDEA so a couple of drops of water were added and boiled for a few more minutes until all of the MDEA had dissolved. Some IPA was boiled off, then the beaker was covered with plastic wrap and placed in the freezer. The yield after recrystallization was 7.7 g.
Min danske:
10 g sølvpapir blev strimlet og placeret i en 1 liters kolbe, 3 udgange,RBF. 300 ml MeOH med en
smule Mercuric Thiocyanate blev tilsat [et hvert mercuric salt kan bruges] og en blanding var begyndt.
i en ekstern trakt var der placeret 10 g yummy gul MPD-2-P, 10 ml nitrophane
hvilken kan købes hos en issenkræmmer, og 30 ml. Methanol.
Da sammensmeltningen havde fundet sted, var Ketone/Etno2 begyndt at dryppe med dryp i sekundet indtil reaktionen var gået voldsomt.
Så bar dryp farten ændret til holde reaktionen voldsom, men ikke ude
af kontrol. omkring 15 min er anbefalet for den eksterne. Varme var anvnedt til at opretholde et tilbageløb. Omkring halv anden time efter, blev kolben nedkølet til stue temperatur og 300 ml. 35% NAoH, som var ned kølet til omkring 0°C var tilført. Den mørke grå, næsten sorte væske blev
ekstraheret 4 gange i Toluene.
toluene ebkstraktionen blev kombineret, vasket med vand 4 gange og en gang med salt vand. et par klumper af bagt epsom salte var tilført til toluenen. Og det var i fryseren et stykke tid. Det forfærdelige HCL gasnings apparat var samlet, toluenen desileredes fra epsom saltene, og bobblede med tør HCL gas. Bundfaldet var filtret og toluene gasset noget mere og mere bundfaldvar filtreret, så blev toluenen gasset, og der var intet bundfald. Bundfaldet blev vasket med anhydrous acetone og luft tøret.
Vægt, 8.8 g.
Rekrystalisering var forsøgt med 63 ml acetonitrile, hvilket ville have virket perfekt med MDMA, men næsten intet af MDEA`en ville opløses, ikke engang ved kogning. Endnu 63 Ml var tilført og bragt i kog. Men det meste pulver der var tilbage var uopløst. Acetonitrilen var nedkølet og MDEA var filtreret. acentonitrile var --- i forhold til MEDA`en i kolben.
Rekrystalisering var forsøgt igen med Isopropyl alcohol. 350 ml kogende IPA havde stadig ikke opløst alt MDEA`en, så et par dråber vand var tilført og kogt i et par minutter indtil alt MDEA var opløst. Noget IPA var kogt væk, så blev bægeret dækket med husfilm, og placeret i fryseren.
Udbyttet efter rekrysalliseringen var 7.7 g.
Steder hvor der står --- betyder at jeg ikke på nogen måde ved hvad det er eller betyder.
Vil oss mene at rekrystaliseringen er temmelig klumpe-dumpet..
Kan det ikk gøres nemmere ?
-Tramperen-
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