Sinteza 4mmc z etil acetatom v 20min

G.Patton

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Pri tej reakciji nastane Br2. Ko je prostornina Br2 prevelika, se reakcija ustavi.
 

baadwd332

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> Br2 forms during this reaction.
bromine is not created during amination.
 

G.Patton

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Where it's going in your opinion?
 

baadwd332

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Br- ions, or - in theory - CH3NH2 * HBr (which dissociate to CH3NH3+ and Br- in water that is already there).
If there would be Br2 you would smell it for sure :)
 

StarWars

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Potem u uporabite toulen benzen dcm ni enako kot pri etilacetatu?
 
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TheVacuumGuy

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DCM bi moral biti tu 3L.

Etil acetata lahko uporabite manj
 

dvmian55

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czesc. mozesz mi napisac dokladna nazwe sprzetu ? dopiero zaczynam wiec wole postawic na bezpieczenstwo a reakcja wydaje sie prosta na poczatek i bede mogl popracowac z krystalizacja od razu :)
 

dodobird

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I'm confused which video is this exactly?
 

Chemix-Express

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Imam nekaj temeljnih vprašanj:
1. Ali pred dodajanjem m40 ne segrejemo vsega na 40 stopinj, temveč dodamo ves m40 naenkrat?
2. pri dodajanju m40 ni treba paziti na temperaturo?
3. ali lahko za zakisanje namesto hcl + aceton uporabim HCL + IPA? Želel bi se znebiti nepotrebne barve pri kisanju.
4. izkoristek je bil manjši zaradi uporabe jodo ketona, z bk4 bi moral biti boljši?
5. v videoposnetku na forumu piše, da se reakcija konča, ko je baza rjava, tudi pri bk4? Ali obstaja kakšen drug način za potrditev, da je reakcija v celoti potekala?

Hvala za vaš čas
 
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TheVacuumGuy

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Ne poskušam vas popravljati, ampak se trenutno učim in preizkušam enačbe. Zato bi lahko potrdili naslednje:

C10H11BrO + CH3NH2 = C11H15NO + HBr

Kar bi pomenilo, da nastane HBr, saj je Br2 dvoatomni?

Chemix Žal mi je, da je bilo to vprašanje za G.patton
 

dodobird

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Please confirm that when using 2b4m as precursor, the freebase oil will be deep dark yellow ideally and not brown. Will be appreciated
 

Mellym

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Za tiste, ki jih to zanima. Poskusil sem to pot. Na splošno lahko potrdim, da deluje, razen reakcijskih pogojev. Temperatura in čas nista bila niti približno takšna, kot je navedeno v videoposnetku. Čeprav v videoposnetku uporabljajo jodo-keton. To je precejšnja razlika.
Tako sem pri testni izvedbi dobil 50 g bromovega nadomestka 4-MPF. To je bilo raztopljeno v 250 ml etilacetata

nato je bilo dodanih 100 ml 38-odstotnega metilaminskega vodika in puščeno, da se meša pri sobni temperaturi:
KodTGgMOq9

Po približno 30 minutah se ni veliko spremenilo:
D6jlCeSBds
V tem trenutku sem se odločil, da stvari segrejem. Ne več kot 50-55C.

Po eni uri:
SH1aVcQCEZ
Pokazalo se je nekaj gibanja. Pustili smo ga še eno uro.
Potem so bili koraki v bistvu enaki kot v videoposnetku. Etilacetatna plast s prosto bazo je bila ločena, sprana z vodo, HCL je bila dodana po kapljicah do rahlo kislega pH. Nato se vlije aceton in filtrira.
MoFsHzIBZ8 0nutxPTB3j I1kq97R3Ow
Tako je nastal surovi izdelek. Na prvi pogled precej lep, vendar bi ga bilo treba seveda dodatno očistiti.
 

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StarWars

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Uporabljate preveč etil acetata, morate uporabiti samo 100 ml, ne 250 ml.
 
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TheVacuumGuy

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Ja. Za razliko od drugih topil, pri katerih lahko v grobem uporabite količino x 3, je pri tem topilu količina x 2.
100 g ketona
200 ml etil acetata
200 ml metilaminu
Brez toplote je bs, samo nežna toplota rm 30c
Dodajte amin, ni potrebe po kapljicah, dodajte ga naravnost, vendar ne pretiravajte.
Temperatura bo narasla na 50/60 in se počasi ohladila. Barve so svetlo rumena, temnejša rumena, očiščena rumena, očiščena temno rumena. Pripravljeno

Zelo dobra pot, brez vonja po aminu kot pri DCM, in lahko se odstrani v stranišče.
Nekajkrat sem to naredil tudi v dnevni sobi brez težav.
 
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dvmian55

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te skladniki po prostu musze wymieszac ?
 

PersonVPN

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Hi Bro!
Pls. Use English.
 

William D.

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It is better to use x4 of ethylacetate, because part will be lost when washing
 

dodobird

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Please explain this step if 4 x ea ..why that matters with respect to future reactions and final product yield?
Why we need extra ea when it should rather be removed before acidification

Noobie question but an answer will be greatly appreciated, friends. 😀😃
 

dodobird

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Hi there .. after acidification did you cover the slurry solution and put in the fridge or freezer and the wash with acetone and dry?

Temperature and duration please 🙏
 
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