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Metamfetamino sintezė iš efedrino naudojant I2 ir H3PO2

GhostChemist

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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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Labai ačiū už pasidalijimą. Dar viena klasikinio preparato gija sukuria puikų etapą naujokams.
 

hacke8

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Yra keli paprasti klausimai: 1. Ar galima naudoti 99 % hipoforinę rūgštį? 2: Kokia yra geriausia specifinė refliukso temperatūra? 3: Kokį katalizatorių galima įdėti, kad reakcija vyktų greičiau, nelaukiant 10-12 val. 4: Ar garinant DCM galima pirmiausia filtruoti natrio sulfatą, kad būtų galima valdyti kitus etapus?
 

GhostChemist

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1. yep
2. 100-160 C
3. Dabar procesas be katalizatorių (gali būti ateityje)
4. nesuprantu šio klausimo
 

hacke8

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Ponai, atlikau šį eksperimentą ir kaitinau iki 125 laipsnių, nes fosforo rūgštį įkaitinus iki 130 laipsnių, atsiras fosfatinio vandenilio dujų (nuodingos). Ar yra koks nors būdas jų išvengti?
 

billythekid

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Tai hipofosforo rūgštis, o reakcijos mišinį kaitinant daugiau nei 110 atsiranda didesnis priemaišų kiekis ir yra pavojinga nenorite skaidyti hipo didelė gaisro sprogimo ir apsinuodijimo rizika kantrybė svarbu čia
 
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hacke8

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Taip, pone, aš naudoju 50 % H3PO2, o ideali temperatūra neviršija 110 laipsnių, tiesa?
 

billythekid

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110 laipsnių pagal Celsijų yra geriausia, kaip man atrodo, bet 130 laipsnių temperatūroje jis skyla į fosfino dujas (savaime užsidegančias) ir fosforo rūgštį, nes turėti sandarų grįžtamąjį kondensatorių nėra gera idėja, mažesnėms reakcijoms galite viršuje uždėti balioną, kad padėtų išlaikyti vandenilio dujas,
 

hacke8

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Taip, pone. Taip pat ant kondensatoriaus sumontavau du didelius balionus, kad būtų galima patalpinti jodo išgaravimą. Kiek laiko užtrunka metilo konversija 110 laipsnių temperatūroje?
 

GhostChemist

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galite naudoti PH3 absorbciją su NaClO ir NaOH
H3PO2 sunaikintas 170 C temperatūroje
 

hacke8

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Sveiki, pone, šitas prakeiktas vertimas, nesuprantu, ką turite omenyje. Turite omenyje kokį natrį ar dar ką nors? Kaip veikia natris? Ačiū už atsakymą.
 

CARLITOBRO

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ar galiu vietoj hipofosforo rūgšties naudoti 57% hidriodinę rūgštį ? prašom pakartoti
 

Mr.blank00

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Laba diena, pone, ar viršutinis kondensatoriaus dangtelis atidaromas ar uždaromas, kai refliuksuojama 10-12 valandų, ir ar kondensatoriui aušinti naudojamas ledinis vanduo, nes jei 12 valandų tiesiog kaitinsite be kondensatoriaus, tirpalas išgaruos ir išdžius, paaiškinkite.
 

hacke8

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Sveiki, ar žinote, kodėl jis vadinamas kondensatoriumi, o ne kitu pavadinimu?
 

GhostChemist

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grįžtamasis kondensatorius turi būti atidarytas arba uždengtas vandenyje išmirkytu vatos gabalėliu
 

hacke8

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Reikia šalto vandens, kuo šaltesnio, tuo geriau, nes sandariklyje gali įvykti sprogimas.
 

ImRegistered

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Ar ši sintezė veiktų su p2p ?
 

hacke8

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Ne, tai tinka tik efedrinui. P2P naudojama amalgama arba kitos linijos.
 

hacke8

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Taip, yra daugybė būdų pasirinkti jums tinkamą BB forumą.
 

hacke8

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Pone, nesuprantu nė vieno žingsnio. 17 paveiksle DHM distiliuojamas 90-110 laipsnių temperatūroje. Kas yra tas DHM? O gal jis gali būti distiliuojamas tiesiai 40 laipsnių temperatūroje ir neišsilieti?
 
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