Süntees 4mmc etüülatsetaadiga 20min jooksul

G.Patton

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Selle reaktsiooni käigus moodustub Br2. Kui Br2 maht on liiga suur, reaktsioon peatub.
 

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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Siis u kasutada toulen benzen dcm ei ole sama nagu etüülatsetaat??
 
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TheVacuumGuy

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Tbh DCM peaks siin olema 3L.

EthylAcetate võite kasutada vähem
 

dobrytowar55

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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?
 

whitelabel

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How much crystal mass you get from 1kg bk4?
 

Chemix-Express

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Mul on paar põhimõttelist küsimust:
1. Kas me ei kuumuta kogu asja enne m40 lisamist 40 kraadini ja lisame kogu m40 korraga?
2. m40 lisamisel ei ole vaja jälgida temperatuuri?
3. kas hcl + atsetooni asemel võib kasutada HCL + IPA hapestamiseks? Tahaks hapendamisel vabaneda mittevajalikust värvist.
4. saagis tuli väiksem tänu joduketooni kasutamisele, bk4-ga peaks olema parem?
5. foorumi videos on kirjas, et reaktsioon lõpeb kui alus on pruun, bk4-ga ka? Või on mingi muu võimalus kinnitada, et kogu on täielikult läinud?

Tänud aja eest
 
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TheVacuumGuy

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Ei püüa teid parandada, vaid õppida ja proovida võrrandeid hetkel. Nii et kas te saaksite kinnitada järgmist:

C10H11BrO + CH3NH2 = C11H15NO + HBr

Mis tähendaks, et HBr moodustub, kuna Br2 on kaheaatomiline ?

Chemix sorry see oli küsimus G.pattonile
 

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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Neile, kes on huvitatud. Ma olen seda teed proovinud. Üldiselt võin kinnitada, et see toimib, välja arvatud reaktsioonitingimused. Temperatuur ja ajastus ei olnud isegi lähedased, nagu on märgitud videos. Kuigi, videos kasutavad nad jodo-ketooni. See on oluline erinevus.
Niisiis, proovisõidu sain 50g bromi asemel 4-MPF. See lahustati 250ml etüülatsetaadis.

kui 100ml aq. 38% metüülamiini lisati. ja jäeti segada toatemperatuuril:
KodTGgMOq9

Umbes 30 min. pärast ei olnud palju muutunud:
D6jlCeSBds
Sel hetkel otsustasin asju soojendada . Mitte kõrgemale umbes 50-55C.

Üks tund hiljem:
SH1aVcQCEZ
See näitas mõningast liikumist. Ja jäeti veel tunniks.
Siis olid põhimõtteliselt samad sammud nagu videos. Etüülatsetaat kiht koos vabalahusega eraldati, pesti veega, HCL lisati tilkhaaval kuni kergelt happelise pH-ni. Seejärel valati atsetooni ja filtreeriti.
MoFsHzIBZ8 0nutxPTB3j I1kq97R3Ow
Ja see andis toorainet. Esmapilgul üsna kena, kuid tuleks muidugi edasi puhastada.
 

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StarWars

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U kasutada liiga palju etüülatsetaat u vaja kasutada ainult 100ml ei 250ml
 
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TheVacuumGuy

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Jah. Erinevalt teistest lahustitest, mida saab kasutada umbes x 3 koguses, on see x 2.
100g ketooni
200ml etüülatsetaat
200ml metüülamiini
Kuumust ei ole bs, lihtsalt õrnalt kuumutada rm 30c
Lisa amiin, ei ole vaja tilgutada, lihtsalt lisa otse, aga mitte üle pingutada.
Temperatuur tõuseb 50/60 ja jahtub aeglaselt. Värvid on helekollane , tumekollane, selgunud kollane, selgunud sügav tumekollane. Valmis

Väga mõnus tee, ei ole amiinilõhna nagu DCM ja seda saab hävitada WC-sse.
Ma teen seda isegi elutoas paar korda ilma probleemita
 
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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. 😀😃
 

William D.

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You can take less ethylacetate, enough for BK4 to be dissolved. The reaction when stirring can be very hot, which will benefit if you do not have the ability to heat with a hot plate and a hot bath. But when you collect the product, EA may not be enough to collect all the base from the reaction mixture and wash the methylamine with water without loss for the product. Then we can use an additional portion of EA at the end of the reaction for extraction. Or another solvent. The next stage, when we make acidification in the EA and if we use aq. acid, it is better to cool the EA with the base and hold the temperature with the whole process. Then your yield will be more.
 

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 🙏
 

BalkanBoys

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So you can use bromoketone instead if iodoketone and still use Ethyl acetat as a solvent instead of N-methylpirolldone like its shown in the video ? Because in Bromoketon video NMP is used and iodoketone Ethyl acetat is used. I can get ethyl acetat 10l for 40 dollars. So can i do Bromoketon way and use EA instead of NMP ?
 
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