Sinteza mefedrona (4-MMC) iz haloketona v etil acetatu. 1-10 kg Lestvica.

[William D.]

Reaction scheme:

​

Reagents:
1. 4'-Methylpropiophenone (cas 5337-93-9) 1 kg;
2. Hydrobromic acid 48% 1300 ml;
3. Hydrogen peroxide 35% 750 ml;
4. Sodium/potassium hydroxide 25% (NaOH/KOH) aqueous solution;
5. Distilled water;
6. Ethyl acetate 6 l;
7. Methylamine 40% aq - 2 l;
8. Acetone - 8 l;
9. Hydrochloric acid (HCl 38%) 500 ml;
10. Isopropyl alcohol;

Equipment and glassware:
1. Scales;
2. Jacketed 10 L reactor equipped with reflux condenser, drip funnel, thermometer, top stirrer and temperature control system;
3. Heating pump;
3. Chiller pump;
4. Vacuum source;
5. Buckets;
6. Freezer;
7. Pyrex dishes;
8. Nutsche filter;
9. pH indicator papers;

Stage 1. Halogenation

​

1. 4'-Methylpropiophenone 1000 g is added into a 10 L reactor flask.​

2. Hydrobromic (HBr) acid 1300 g 48% is poured into the flask and stirred for 5 min.
3. Hydrogen peroxide 750 g 35% is added into a drip funnel 1 l.
4. Hydrogen peroxide is added dropwise to the stirred reaction mixture.
5. Bromine is released during hydrogen peroxide addition to the mixture, dissolved in solution and reacted.
6. Hydrogen peroxide must be added at an appropriate rate so that the reaction mixture becomes colorless.
7. Reaction mixture temperature have to be kept less than 65 °C. An external cooling is applied in case of overheating. If reaction temperature is higher, hydrogen peroxide addition is stopped.
8. The second part of discoloration reaction can be conducted for longer time. Hydrogen peroxide is added according with reaction temperature.
9. Reaction mixture is left for a 12 h with a constant stirring at room temperature as soon as all hydrogen peroxide is added.
10. After 12 h precipitate is formed.
11. Sodium bicarbonate aq solution is added to the reaction mixture to reach neutral pH 6-7, stir it well. The mixture with 2-bromo-4'-methylpropiophenone is filtered through a Buchner funnel. Product is washed with small amount of distilled water.
12. Crude 2-bromo-4'-methylpropiophenone (cas 1451-82-7) is used for further reactions. Theoretical yield up to 1530 g. Practice yield is almost quantitative (video yield 94%).

13. The resulting product is left in the reactor.​

Stage 2. Methamination.

​

1. Ethyl acetate 6 l is poured into the reactor.
2. Reaction mixture is stirred and heated in Jacketed reactor up to 30 °C with help of heating system.
3. The mixture is stirred until complete amount of 2-bromo-4'-methylpropiophenone (cas 1451-82-7) is dissolved.
4. Methylamine 40% aq 2 l is added at once.
5. The mixture is stirred for 20 min, temperature is kept below 65 °C.
6. The stirring is stopped. The reaction mixture is left for layer separations. A bottom layer is drained through a bottom reactor tap..
7. After that, the mixture is heated up to 55 °C and reactor vacuum pump is turned on. The reactor condenser chiller pump is turned on as well.
8. All amount of ethyl acetate or the biggest part of it is distilled off.
9. Vacuum pump is turned off. Acetone is added to the reactor with a constant stirring.
10. Hydrochloric acid (500 ml) is placed into the drip funnel and the funnel is installed onto the reactor neck.
11. Hydrochloric acid is added dropwise to reach pH 5 with constant stirring. A small amount (~2-5 ml) of reaction mixture is drained from the bottom reactor tap in order to check pH by pH indicator stripe. The sample is poured back into the reaction mixture.
12. After that, the mixture is poured into a bucket and the bucket is put into a freezer for 12 h.

Download Video

Mephedrone synthesis

• Novator
• Apr 6, 2023
• 100
• 2-iodo-1-p-tolyl-propan-1-one 2-iodo-4'-methylpropiophenone 4-mmc cas 236117-38-7 meph mephedrone mephedrone hydrobromide mephedrone hydrochloride mephedrone video synthesis

Mephedrone synthesis from 2-iodo-4'-methylpropiophenone (CAS 236117-38-7) with ethyl acetate...

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Stage 3. Filtration.
1. A vacuum filtration system (Nutsche filter, filter cloth, vacuum pump) is assembled and installed.
2. The vacuum pump is turned on.
3. A bucket content from step 12 stage 2 is poured to the Nutsche filter.
4. The mixture is filtered and pressed until the funnel content is become solid.
5. A cold dry acetone is poured onto the solid product in the funnel in several small portions during filtration.
6. Acetone is filtered. Step 5 is repeated, if the solid is not white.
7. White solid 4-MMC product is moved into a Pyrex dish for a drying after filtration procedure.
8. Pyrex dish with 4-MMC is placed into a dry well ventilated warm room.
9. 4-MMC product is dried to a constant mass. Product is mixed and grinded periodically in order to increase drying speed.

Stage 4. Recrystallisation.
Mephedrone (4MMC) crystallization

 

[woohoo]

Ali ga ni bilo treba ločiti od n-metilacetamida?
Zdi se, da je njegova reakcija umazana, koliko daje v primerjavi z nmp ali aromatskim topilom?

 

[yin-yang]

N-metilacetamid naj bi bil topen v acetonu, čeprav nisem našel, koliko. Freebaza je res črna, dobljeni prah pa ob dodatku kristalizacijske mešanice topil postane zelen (nereagirani keton?). Lahko sklepamo, da to ni najbolj čist postopek.

Nekateri prisegajo, da je pri kateri koli drugi reakciji razen tiste, pri kateri se kot topilo uporablja NMP, končni izdelek veliko, veliko slabši. Več hitrega vzburjenja brez evforije.

Ali ste izvedli GC-MS, da bi ugotovili, ali so v dobljenem prahu/kristalih kakšne nečistoče?
@G.Patton
@Marvin "Popcorn" Sutton
@William Dampier

 

[Wan Jack]

(6.The stirring is stopped. The reaction mixture is left for layer separations. A bottom layer is drained through a bottom reactor tap..)Because of the excess methylamine, the free base was washed more than 3 times with more than 2 times the deionized water.

 

[G.Patton]

Pozdravljeni, verjetno ste naredili nekaj narobe ali pa vaši reagenti niso tako dobri. Da, opravili smo GC-MS. 96,4 % 4-MMC

 

[yin-yang]

Te reakcije še nisem preizkusil. Ogledal sem si videoposnetek, objavljen tukaj jodoketonska aminizacija. Tam sem videl, da je prosta baza črna, prah pa je med pripravo za kristalizacijo spremenil barvo. Morda je bil črn zato, ker je jod v nasprotju z bromom izstopajoča skupina.
Vprašanja za potrditev:

1. Zgornji rezultati so iz etil acetata kot topila?
2. Ali ste to reakcijo izvedli z EA in bromoketonom, ali je prosta baza videti drugače?
3. Na videoposnetku sem opazil, da so kristali iz EA videti kot steklo, medtem ko so pri NMP veliko bolj beli. 4. Prebral sem vaš prispevek o stereokemiji 4-MMC, kako enantiomera S in R tvorita kristale različnega videza, sta oba kristala enako racemična?
4. Ali ste opazili kakšno razliko v subjektivnem učinku med EA in recimo NMP v končnem izdelku?

Zahvaljujem se vam za objavo teh rezultatov.

 

[DavidNichols]

Ali me lahko prosim povežete na to delovno mesto?

 

[G.Patton]

Pravzaprav se ne spomnim zagotovo. Verjetno da.
Da, to so racemični kristali.
Kot vsak dober proizvajalec vina izdelka nisem poskusil =)

 

[StarWars]

8. Nato zmes segrejemo na 55
v videoposnetku jasno piše, da ni treba segrevati. tu pa je nekdo napisal, da se nato segreje za kaj, če zmes sama doseže temperaturo, ki ni višja od 65 °.

 

[G.Patton]

Pozdravljeni, 55 stopinj *C je potrebnih za vakuumsko izparevanje topil in presežka metilamina. To je neobvezen postopek.

 

[goku1008]

can i skip this i dont have vacuum systume
and plz give me your screenshot video link plz

 

[G.Patton]

This video in the topic, dude...
Yes, you can separate layers without vacuum. There is this information in the screenshot.

 

[Chemix-Express]

Ta sinteza me zelo zanima, čez nekaj dni jo bom imel priložnost preizkusiti, zato imam nekaj vprašanj:
V koraku 2, točka 10, lahko namesto acetona uporabim IPA? Ko uporabim HCL 35-37 % aq v kombinaciji z acetonom, je vedno veliko barve, 1,4-dioksan je pomagal, vendar je zelo drag. Ali menite, da bo IPA deloval?
2. V točki 5 faze 2 je navedeno, da je treba dodati ves m40 naenkrat, v točki 6 pa je navedeno, da je treba temperaturo vzdrževati pod 65 °C. Ali lahko temperaturo nadzorujem s postopnim dodajanjem m40 ali nujno z zunanjim hladilnikom?
3. Ali naj reakcijski čas (20 minut) štejem od trenutka, ko končam dodajanje m40?
4. Zanima me, zakaj je tako malo informacij o sintezi 4MMC v etil acetatu, ko niti na začetku niti med reakcijo zmesi ni treba segrevati, sam etil acetat pa je zelo poceni. Ali temu sledi majhen izkoristek/čistost reakcije?
5. Če skrajšamo, ali bi bilo razmerje 1 kg bk4, 2 l m40, 2 l etil acetata dobro ali je bolje, da za vsak kg bk4 dobimo 1,5 l m40 in 2,5 l etil acetata?

 

[little-flower]

Ali lahko to reakcijo izvedemo z 12 % H202? Mislim, da je morda dobra.""

 

[StarWars]

U lahko naredite

 

[Rush-Benzo]

Kolikšna naj bi bila količina pripravljenega reagenta BK4, če ga uporabim za 2L m40?

 

[G.Patton]

Pozdravljeni, količino reagentov lahko sorazmerno povečate. Preberite temo o molih, gramih, litrih in kemijskih izračunih.

 

[xoxo2.0]

to je 1000. rezultat reakcije @G.Patton

 

[Rush-Benzo]

Govoril sem o nečem povsem drugem. Ne vem, koliko končnega BK4 ste dobili po končani prvi fazi. Začeti želim od faze 2 in ne vem, koliko BK4 naj uporabim. Koliko ste ga dobili po končani stopnji 1.

 

[G.Patton]

Približno 1350-1450 g 2-bromo-4'-metilpropiofenona iz prve faze.

 

[Rush-Benzo]

Najlepša hvala.

Če to ni težava, bom postavil še eno vprašanje. V 2. koraku, točka 9, pravite, da je treba destilirati vsaj polovico etil acetata, kaj naj bi to pomenilo? V videoposnetku z navodili je navedeno, da je ta korak neobvezen. Ali bom z opustitvijo tega postopka izgubil učinkovitost, kakovost ali pa mi bo to le olajšalo delo z manjšo količino tekočin?

Trenutno kupujem zmogljivo vakuumsko črpalko, iz radovednosti pa bom vprašal, koliko časa traja destilacija teh 6 l etil acetata, ki se segreje na 55 stopinj?

 

[StarWars]

Oglejte si videoposnetek, če uporabimo 1 kg bk4, potrebujemo 2 l etil acetata in 2 l metilomina.
Tam na videoposnetku prodajajo 6 l, haha

 

[G.Patton]

>>>V točki 9 drugega koraka pravite, da je treba destilirati vsaj polovico etil acetata, kaj naj bi to pomenilo?
To je potrebno za kristalizacijo vašega mefedrona.
>>> Ali bom z opustitvijo tega izgubil učinkovitost, kakovost ali mi bo to le olajšalo delo z manjšo količino tekočin?
V vsakem primeru ga boste destilirali, bolje je, da to storite na tej stopnji, da bi dobili večji izkoristek med dodajanjem HCl.

 

[StarWars]

daš na električni štedilnik in po pranju izhlapi 50% topila, vendar je v tem videu še vedno veliko napak. čistiš 1x voda + soda nato 3x voda nato izhlapi 50% nato dodaš magnezijev solfat, da ne izgubiš produkta in zakisiš in to je to. Na starem prenosnem računalniku imam podoben videoposnetek, v katerem namesto etil acetata uporabljajo dcm. Po mojem mnenju je izhlapevanje nesmiselno, naredil sem brez njega in pri sintezi ni bilo težav.

 

[G.Patton]

Kakšen izkupiček ste dobili? Enak?