Síntesis 4mmc con acetato de etilo en 20min

G.Patton

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Durante esta reacción se forma Br2. Cuando el volumen de Br2 es demasiado grande, la reacción se detiene.
 

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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Entonces u uso toulen benzen dcm no es lo mismo como en acetato de etilo??
 
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TheVacuumGuy

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Tbh DCM debería ser 3L aquí.

El acetato de etilo puede ser menor.
 

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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Tengo un par de preguntas fundamentales:
1. ¿no calentamos todo a 40 grados antes de añadir el m40, y añadimos todo el m40 a la vez?
2. ¿no es necesario vigilar la temperatura al añadir m40?
3. ¿puedo utilizar HCL + IPA para la acidificación en lugar de hcl + acetona? Quiero eliminar el color innecesario al acidificar.
4. el rendimiento fue menor debido al uso de yodo cetona, ¿con bk4 debería ser mejor?
5. en el video del foro dice que la reacción termina cuando la base es marrón, ¿con bk4 también? ¿O hay otra forma de confirmar que el conjunto se ha completado?

Gracias por vuestro tiempo
 
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TheVacuumGuy

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No intento corregirte, pero estoy aprendiendo y probando ecuaciones. Entonces, ¿podría confirmar lo siguiente?

C10H11BrO + CH3NH2 = C11H15NO + HBr

¿Lo que significaría que se está formando HBr ya que el Br2 es diatómico?

Chemix lo siento esta era una pregunta para 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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Para quien esté interesado. He probado esta ruta. En general puedo confirmar que funciona, excepto las condiciones de reacción. La temperatura y el tiempo no eran ni siquiera cerca como se indica en el video. Aunque, en el video que utilizan yodo-cetona. Esa es una diferencia significativa.
Así que, en la prueba de funcionamiento conseguí 50g de 4-MPF sustituido por bromo. Eso se disolvió en 250ml de etilacetato

que 100ml de aq. 38% de metilamina se añadió. y se dejó agitar a temperatura ambiente:
KodTGgMOq9

Después de unos 30 minutos no había cambiado mucho:
D6jlCeSBds
En este momento decidí calentar las cosas . No más alto unos 50-55C.

Una hora más tarde:
SH1aVcQCEZ
Estaba mostrando algo de movimiento. Y se dejó durante otra hora.
Entonces básicamente los pasos fueron los mismos que en el vídeo. Se separó la capa de etilacetato con la base libre, se lavó con agua, se añadió HCL gota a gota hasta conseguir un pH ligeramente ácido. Luego se vertió acetona y se filtró.
MoFsHzIBZ8 0nutxPTB3j I1kq97R3Ow
Y eso dio producto en bruto. Bastante agradable a primera vista, pero debe ser purificado aún más, por supuesto.
 

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StarWars

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Utilizas demasiado acetato de etilo, sólo necesitas 100 ml y no 250 ml.
 
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TheVacuumGuy

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Sí. A diferencia de otros disolventes de los que puedes utilizar aproximadamente una cantidad x 3, éste es x 2.
100g de cetona
200 ml de acetato de etilo
200ml de metilamina
Sin calor es bs, sólo calor suave rm 30c
Añade la amina, no hace falta que sea gota a gota, añádela directamente, pero sin pasarse.
La temperatura subirá a 50/60 y se enfriará lentamente. Los colores son amarillo claro, amarillo oscuro, amarillo aclarado, amarillo oscuro aclarado. Hecho

Es una ruta muy agradable, no huele a aminas como el DCM, y se puede desechar en el inodoro.
Yo lo hago incluso en la sala de estar par de veces no hay problema
 
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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.
 

Come on 666

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What is the final effect of your product?
I also think that 100 grams of 2-bromo-4'-methylpropiophenone is added to 400 ml of ethyl acetate,Then add 40% aqueous solution of methylamine,It is impossible to react successfully within 20 minutes.
The reaction should be successful at 40℃ for 2 hours
What do you think?
 

dodobird

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30 mins but acidification issues using ethyl Acetate. Dcm is the easiest
 

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 ?
 

prvnc

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The short 20-minute mix/shake without heating likely relies on reactive precursors and a catalyst (M40%) to speed up the reaction. Heating isn’t always necessary if the reaction is exothermic or efficient at room temperature. Purity depends on reactant quality and workup, but expect moderate to high purity with proper purification. Using a closed borosilicate bottle is possible to contain vapors and maintain pressure, but ensure safe ventilation and avoid overpressure risks. Always prioritize safety and verify reaction specifics before scaling up.
 
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