Sinteza metamfetamina iz efedrina z uporabo I2 in 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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Najlepša hvala za delitev. Še ena klasična nit za pripravo ustvarja odlično prizorišče za novince.
 

hacke8

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Obstaja nekaj preprostih vprašanj, 1: Ali je mogoče uporabiti 99-odstotno hipoforno kislino? 2: Katera je najboljša specifična temperatura refluksa? 3: Kakšen katalizator lahko dodamo, da reakcijo pospešimo, ne da bi čakali 10-12 ur. 4: Ali lahko pri izparevanju DCM najprej filtrirate natrijev sulfat, da bi delovali v naslednjih korakih?
 

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1. yep
2. 100-160 C
3. Zdaj postopek brez katalizatorjev (morda v prihodnosti)
4. ne razumem tega vprašanja
 

hacke8

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Gospodje, naredil sem ta poskus in ga segrel na 125 stopinj, ker se fosforjeva kislina segreje na 130 stopinj, nastane fosfatni vodikov plin (strupen). Ali obstaja kakšen način, da se temu izognemo?
 

billythekid

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To je hipofosforna kislina in segrevanje reakcijske mešanice nad 110 povzroči večjo količino nečistoč in je nevarno ne želite razgraditi hipo velika nevarnost požara eksplozije in zastrupitve potrpežljivost je pomembna tukaj
 
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hacke8

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Da, gospod, uporabljam 50 % H3PO2, popolna temperatura pa je znotraj 110 stopinj, kajne?
 

billythekid

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110 stopinj Celzija je po mojem mnenju najbolje, vendar se pri 130 stopinjah razgradi v fosfinski plin (samovnetljiv) in fosforno kislino, ker imeti zaprt povratni hladilnik ni dobra zamisel, za manjše reakcije lahko čezenj postavite balon, ki pomaga zadržati hidrojodni plin,
 

hacke8

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Da, gospod. Na kondenzator sem namestil tudi dva velika balona, da bi namestil izhlapevanje joda. Koliko časa je potrebno za dokončanje pretvorbe metila pri 110 stopinjah?
 

GhostChemist

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lahko uporabite absorpcijo PH3 z NaClO in NaOH
H3PO2 se uniči pri 170 C
 

hacke8

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Pozdravljeni, gospod, ta prekleti prevod, ne razumem, kaj želite povedati. Ali imate v mislih kakšno vrsto natrija ali kaj drugega? Kako deluje? Hvala za odgovor.
 

CARLITOBRO

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ali lahko namesto hipofosforne kisline uporabim 57-odstotno hidriodno kislino ?
 

Mr.blank00

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Pozdravljeni gospod, ali je zgornji pokrov kondenzatorja odprt ali zaprt, ko se refluksira 10-12 ur, in ali se za hlajenje kondenzatorja uporablja ledena voda, ker če se 12 ur samo greje brez kondenzatorja, bo raztopina izhlapela in se posušila, prosim za pojasnilo.
 

hacke8

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Pozdravljeni, ali veste, zakaj se imenuje kondenzator namesto z drugim imenom?
 

hacke8

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Potrebna je hladna voda, čim hladnejša, tem boljša, saj obstaja možnost eksplozije v tesnilu.
 

ImRegistered

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Ali bi ta sinteza delovala s p2p ?
 

hacke8

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Ne, to je primerno samo za efedrin. P2P uporablja amalgam ali druge linije.
 

hacke8

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Da, obstaja veliko načinov za izbiro foruma BB, ki vam ustreza.
 

hacke8

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Gospod, ne razumem niti enega koraka. Na sliki 17 je DHM destiliran pri 90-110 stopinjah. Kaj je to DHM? Ali ga je mogoče destilirati neposredno pri 40 stopinjah, ne da bi iztekel?
 
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