gražus ir efektyvus savarankiškos 2b4m sintezės būdas (vid. 50 JAV dolerių už kg)

[Dr. MMX]

Ei, aš tiesiog įvesiu reagentus, kuriuos naudoja protingas pasirinkimas (kaina / pastangos) aviable to buy in europe
taigi 1.
PCL5 su elementine siera > tionilo chloridas

tionilo chloridas + propiono rūgštis > priopioniklo chloridas

4mp sintezė (čia yra tema, todėl tiesiog pateiksiu nuorodą):
Propionilo chloridas
Toluenas
AlCl3 bevandenis

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/en/threads/synthesis-of-4-methylpropiophenone-from-toluene-by-friedel-crafts-reaction-1kg-scale.209/

kai kurie gali turėti problemų dėl jo bromavimo
sieros rūgštis, kurios reikia norint gauti Hbr, yra šiek tiek brangi ir ne dažnai prieinama. Vietoj to mes naudojame:
fosforo rūgštį ir NaBh reakcijai > gauname HBR
H2O2 12 % galima nusipirkti ir distiliuoti iki 25-30 %.

Taigi
4 metilopropionas + HBR + H2o2 > 2b4m

Neskaičiavau išlaidų, bet jos labai nedidelės ir nereikia laukti siuntos ar būti nustebintam dėl prastos pirmtako kokybės.

 

[chost]

ar galite išsamiau paaiškinti, kaip pagaminti HBR?

 

[Dr. MMX]

Oi labai atsiprašau, kad padariau klaidą. ji teisinga:
Norint iš fosforo rūgšties (H₃PO₄) ir natrio bromido (NaBr) pagaminti hidrobromo rūgštį (HBr), galima naudoti dvigubo išstūmimo reakciją. Reakciją galima pavaizduoti taip:

1. Reagentai: Fosforo rūgštis (H₃PO₄) ir natrio bromidas (NaBr).
2. Produktai: (HBr) ir natrio fosfatas (Na₃PO₄).

Reakcijos subalansuota cheminė lygtis:


H3PO4+3NaBr→3HBr+Na3PO4


Šios reakcijos metu fosforo rūgštis reaguoja su natrio bromidu ir susidaro hidrobromo rūgštis bei natrio fosfatas.

 

[chost]

Ar būtinas distiliavimas?
Ir kokiame kiekyje vandens turėčiau ištirpinti natrio bromidą?

 

[Dr. MMX]

Kaip kitaip planuojate gauti daiktą, kuris iš esmės yra dujos?

Tai priklauso nuo to, kokį % norite turėti, maksimalus yra 47 %, kiek pamenu, ir jis turėtų būti jau toks

 

[Benz88]

is it Safe to Distille the h2o2 to maybe 30-35% from 12%?

 

[TheVacuumGuy]

H3po4 su NaBr gaunamas HBr? Ketinu tai išbandyti po minutės.

Turiu daug HBr, bet tiesiog smalsu, ar šie 2 reaguoja.

 

[Dr. MMX]

taip ir Na3PO4

 

[Dr. MMX]

tai nuostabu

 

[TheVacuumGuy]

Didn't work. I think it would be easier to add sulfuric acid to a solution of KBr (or NaBr) , which would readily yield HBr at 125c

 

[Dr. MMX]

I tried to override having sulfuric acid becasue here is troubles to get it. It was very extreme attempt
if there is access to sulfuric acid its easy job

 

[Dr. MMX]

you can get elemental bromine from potasium bromide, dont need to use acids.
it was quite cheap as i remember

 

[Toddler]

Hbr2 48% can work ?
(CAS.No: 10035-10-6)

how much ration use for bromination
Hbr2
H2O2
for 100g of 4MPP

 

[TheVacuumGuy]

Roughly,

H2o2 50ml
HBr 100ml

 

[Toddler]

for 100g of 4MPP

 

[w2x3f5]

Instead of propionyl chloride, can use propionic anhydride (obtain phosphorus oxide from propionic acid), can also use propionic acid directly with polyphosphoric acid (there are many options for this reaction, you can choose the best one). If propionyl chloride is used with anhydrous aluminum chloride (can be replaced with cheaper and simpler options). Then it is best to carry out a bromination reaction before hydrolysis in Fridel-Crafts (the complex of 2b4m and aluminum chloride is very active for bromination with a high yield).

 

[Dr. MMX]

In chemistry trade buissness in europe propionic acid is considered with "silent restriction" with reason it can be used as biological weapon, so should be avoided there.

very interesting choice of propionic anhydride

 

[Osmosis Vanderwaal]

@TheVacuumGuy you gave him bad figures and he used them and probably ruined 100G 2B4-MP. I dont know what he paid, but I got $200 all day for 10g if it's domestic . In th rules there are a few gold nuggets. "Use the fucking search engine." That's a rule. Another one is " a good chemist i an accurate chemist." Make sure that you clearly state you are guessing when you don't know. You could say nothing at all, you could show your math or you could tell him he needs to figure it himself, but please, dont just throw out random numbers, with no disclaimer.

 

[TheVacuumGuy]

Show me what's wrong then. I used these figures with success. note that hydrogen peroxide is a solution of 35%.

 

[TheVacuumGuy]

i stated roughly , not stoicimeticly

reactants	Coeff	Molar Mass	Moles (g/mol)	Weight (g)
C10H12O	1	148.20168	0,67	100
HBr	1	80.91194	0,67	54,595831842122166
H2O2	1	34.01468	0,67	22,951615663196257
products	1
C10H11BrO	1	227.09774	0.67	153,23560434672535
H2O	2	18.01528	1,35	24,311843158593074

HBr 48% = 8.77 mol/L => for required 0.67m corresponds to 0,0764L (76ml)
h2o2 35% = 11.63 mol/L => for required 0.67m corresponds to 0,0576L (57ml)

Yes that's a bit off from 100 and 50, but these numbers are theoretically, which almost never applies in practice. ( like a mephedrone synthesis is given methylamine x2 but theoretically only needs x1/5 )

furthermore excess reagents are neutralized afterwards.

 

[w2x3f5]

You have not taken into account the purity of precursors, at the end of the reaction you will not have acid. No acid = no protonation

 

[TheVacuumGuy]

.