Metamfetamiini süntees efedriinist, kasutades I2 ja H3PO2

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Starting Reagents and Materials

  • 6 g Synthetic ephedrine hydrochloride racemic
  • 12 g I2
  • 10.8 ml H3PO2 (50%)
  • 20 ml H2O
  • 50 ml 25% NaOH (15-20 г NaOH)
  • 3 g sodium thiosulfate
  • 250-300 ml DCM
  • 30-50 g Na2SO4
  • 100 ml Petroleum ether
  • HCl gas
  • 100 g NH4Cl
  • 25 ml H2SO4 83%
  • Flasks 250 and 500 ml
  • Glasses
  • Funnels
  • Separating funnel
  • Magnetic stirrer with heating
  • Flask heater
  • Reflux
  • Paper filters
  • Pipettes
  • Porcelain filter for vacuum filtration
  • Chen's reagents
  • Simon's reagents
  • pH indicator paper

The process way presented on Scheme 1.
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Starting reagents for meth synthesis: synthetic ephedrine hydrochloride, I2 and H3PO2. Fig. 1
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Ephedrine hydrochloride ground into a powder in a mortar. Fig 2
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The powder of Ephedrine hydrochloride is poured into the flask. Fig 3
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I2 is ground into a powder. Fig 4
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The powder of I2 is to the Ephedrine hydrochloride in the flask and continuously mixing. Fig 5
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The H3PO2 is added in portions to the mixture in the flask while continuously mixing. Fig 6
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The reaction is very intense. Reflux connected to the flask. Fig 7
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The following portions of acid are added after the cessation of the vigorous reaction. Fig 8
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The mixture is heated at a temperature of 100-160°C for 10-12 hours. Fig 9
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The solution should become transparent and homogeneous. Fig 10
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To the resulting reaction mixture, 15-20 ml of water is added. Fig 11
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NaOH solution is added to the RM until reaching an alkaline pH. Fig 12
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Next, sodium thiosulfate solution is added. Fig 13
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The mixture cooled and added 100 ml of DCM (boiling point of DCM is 40°C). Fig 14
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The mixture is transferred to a separating funnel. DCM is separated. Additionally, 2-3 extractions of DCM are carried out with portions of 40-50 ml each. Fig 15
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The layer of DCM is dried with sodium sulfate. Fig 16
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The DCM is distilled at a temperature of 90-110°C until the distillation of DCM ceases. Additionally, sodium sulfate is washed with new portions of DCM. Fig 17
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To the obtained oil, 30+30 ml of petroleum ether is added. Fig 18
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The solution is filtered through a paper filter. Fig 19
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Impurities is in the distillation flask and on the filter. Fig 20
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Solution of methamphetamine in petroleum ether is saturated with gaseous hydrogen chloride until reaching an acidic pH. Hydrogen chloride is generated by adding sulfuric acid to ammonium chloride. Fig 21
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The precipitated meth hydrochloride is filtered. Fig 22
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Simon's reaction with meth hydrochloride is positive (blue coloring); Chen's reaction is negative; Chen's control on a clean sample of ephedrine is positive. Fig 23
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The filtered meth hydrochloride precipitate is dried on the air. Fig 24
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Yield is 4.24 g or 77.1 %
 
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hacke8

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Suur tänu jagamise eest. Veel üks klassikaline ettevalmistusniit loob täiusliku etapi uustulnukatele.
 

hacke8

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On mõned lihtsad küsimused, 1: Kas on võimalik kasutada 99% hüpofoorhapet? 2: Milline on parim spetsiifiline tagasivoolutemperatuur? 3: Millist katalüsaatorit saab lisada, et kiirendada reaktsiooni ilma 10-12 tundi ootamata. 4: Kas DCMi aurustamisel saab kõigepealt filtreerida naatriumsulfaati, et toimida järgmised sammud?
 

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1. Jep
2. 100-160 C
3. Nüüd protsess ilma katalüsaatorita (võib olla tulevikus)
4. ei saa sellest küsimusest aru
 

hacke8

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Härrased, ma tegin selle katse ja kuumutasin seda 125 kraadini, sest fosforhapet kuumutatakse 130 kraadini, tekib fosfaatvesinikgaas (mürgine). Kas on võimalik neid kuidagi vältida?
 

billythekid

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See on hüpofosforhape ja kuumutamine reaktsioonisegu üle 110 toob kaasa suurema hulga lisandeid ja on ohtlik te ei taha lagundada hüpo kõrge tulekahju plahvatuse ja mürgistuse oht kannatlikkus oluline siinkohal
 
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hacke8

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Jah, härra, ma kasutan 50% H3PO2 ja ideaalne temperatuur on 110 kraadi piires, eks?
 

billythekid

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110 kraadi Celsiuse on parim ma leian, kuid see laguneb 130 kraadi juures fosfiingaasiks (iseeneslikult süttiv) ja fosforhappeks, sest tagasivoolukondensaatori kinnipidamine ei ole hea mõte, väiksemate reaktsioonide puhul võite panna ülevalt palli, mis aitab hüdrojoodigaasi sees hoida,
 

hacke8

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Jah. Ma paigaldasin ka kaks suurt õhupalli kondensaatorile, et paigutada joodi lendumine. Kui kaua võtab metüüli muundamine 110 kraadi juures aega?
 

GhostChemist

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saate kasutada PH3 neeldumist NaClO ja NaOH-ga
H3PO2 hävitada 170 C juures
 

hacke8

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Tere, härra, see kuradi tõlge, ma ei saa aru, mida te mõtlete. Kas te mõtlete, millist naatriumi või midagi muud? Kuidas toimida? Tänan teid vastuse eest.
 

CARLITOBRO

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kas ma võin kasutada hüpofosforhappe asemel 57% vesinikkloriidhapet ? palun korrake seda uuesti
 

Mr.blank00

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Tere härra, kas kondensaatori ülemine kaas on avatud või suletud, kui refluksitakse 10-12 tundi, ja kas kondensaatori jahutamiseks kasutatakse jäävett, sest kui seda lihtsalt ilma kondensaatorita 12 tundi kuumutada, aurustub lahus ja kuivab, palun seletage.
 

hacke8

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Tere, kas te teate, miks seda nimetatakse kondensaatoriks mõne muu nimetuse asemel?
 

hacke8

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Vaja on külma vett, mida külmem, seda parem, sest plommis on plahvatusohtlik.
 

ImRegistered

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Kas see süntees toimiks p2p-ga ?
 

hacke8

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Ei, see sobib ainult efedriini jaoks. P2P kasutab amalgaami või muid jooni.
 

hacke8

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Jah, BB-foorumi valimiseks on palju võimalusi, mis teile sobivad.
 

hacke8

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Härra, ma ei saa ühestki sammust aru. Joonis 17, DHM destilleeritakse 90-110 kraadi juures. Mis on see DHM? Või saab seda destilleerida otse 40 kraadi juures, ilma et see välja voolaks?
 
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