Escala de micro-ondas (pequena): 1-fenil-2-nitropropeno (P2NP)

[handle]

Alguém experimentou essa receita exata recentemente? Sei que Jesse_pinkman_ tentou há alguns anos. Mas depois ele entrou em uma tangente com o gálio...

Gostaria muito de ouvir algumas experiências, lições, dicas, ajustes ou truques? Desde já agradeço a todos.

Escala (pequena) de micro-ondas:
1. Benzaldeído 100 ml, nitroetano 100 ml, ácido acético glacial 25 ml e n-butilamina 20 ml são colocados em um béquer de 500 ml.
2. Uma luva de borracha é colocada no béquer.
3. O béquer é colocado em um forno de micro-ondas.
4. A potência do forno de micro-ondas é ajustada para 750 W. O forno é ligado e a mistura é aquecida até a ebulição. A mistura é resfriada até a temperatura ambiente.
5. A etapa 4 é repetida várias vezes. No mínimo 6 vezes.
6. Em seguida, adiciona-se 100 ml de IPA, a mistura de reação é agitada e colocada em um freezer por 12 horas. O 1-fenil-2-nitropropeno(P2NP) é cristalizado.
7. O produto P2NP é filtrado em um funil de Buchner(procedimento de filtração por sucção), lavado com uma pequena quantidade de IPA frio e seco ao ar (ou em câmara de vácuo, opcional).

 

[HIGGS BOSSON]

Fiz pequenas quantidades (até 100 g) no micro-ondas usando esse método e tudo ficou muito simples.

 

[handle]

25 ml de GAA para 20 ml de amina é o melhor? Minha calculadora indicou 40 ml de GAA para 20 ml de amina. Ficarei com 25 ml, a menos que seja aconselhado de outra forma.

 

[chigger18]

i found a way online to make p2p but no one can vitrify it so here it is
"
Today i am wiling to write a nice way for producing P2P without using any controled, expensive or hard obtaining chemicals, all you need is : Iodine, Acetone, Benzene, AlCl3, Copper II Oxide (CuO) and a little chemical glassware.

First, lets prepare our most important reagent: Iodoacetone (its not water soluble, its not strong lachymator as chloroacetone or bromoacetone wich can be used instead of iodoacetone, chloroacetone can be bough comercialy and used instead of iodoacetone, but the yield will be lower. )

First for complete iodination, you will need one mol Acetone per one mol Iodine per one mol Copper II Oxide.
In a 2L flask with magnetic stiring, disolve your Iodine into Methanol, and pour the coper oxide into it, it will create a dork brown solution, once all is disolved add your Acetone and heat for 1,5 hours at 60C, then add a little water , not to form 2 layers, just to make the CuO less soluble in the solution and filter it off. Now you have yellow colored solution, wich is put in destilation aparature and all of the methanol and most of the water are destiled over, then the iodoacetone is washed 2 times with NaCl water solution, and placed in a jar with dry MgSo4 to make anhydrous Iodoacetone. You can skip all that and buy a chloroacetone instead.

Step 2: The reaction.
We are gona acetylate benzene with iodoacetone, with alcl3 as catalyst. (Very important all reagents must be very dry, as alcl3 reacts with water very exotermicaly and will ruin the rection)
The proportions: 1 mole of Iodoacetone is dripped over 1,1mole benzene and 1 mole AlCl3 solution.
While dripping your iodoacetone, you need to cool your reaction flask with ice bath, once the iodoacetone is aded, stop cooling and heat up to araund 50-60C and stir with condenser for 2 additinal hours.

Step 3 : Workup
Put in a flask a lot of ice cubes, add 20ml 37% HCL acid and slowly add your reaction mixture to the flask with the ice and hcl, it will react very exotermicaly and form 2 layers, stir for atlest hour to ensnhure all p2p have been formed, and prepare for a vacum destilation.
Extract your P2P with diethyl ether, stripp off the ether and then destill your P2P. "
hope some one can help me on this <3 love

 

[bigrob]

Vou tentar fazer isso assim que os suprimentos chegarem

 

[Rabidreject]

O problema é que acho que prefiro guardar meu nitroetano para quando meu 3,4,5-TMOBA chegar e eu não quiser muito o p2np a ponto de me dar ao trabalho de obter n-butilamina....mas ouvi dizer que outras aminas volumosas também funcionam... a trietilamina funcionaria?

 

[Rabidreject]

Ooo, isso é interessante...

Eu realmente planejo tentar fazer um pouco de ciclohexilamina...

Eu ia tentar fazer um vídeo sobre isso, já que não há nenhum no YouTube - fiquei surpreso com isso... se eu realmente conseguir fazê-lo funcionar, isto é, rs

Vamos ver, mas, se não conseguir, posso comprá-lo para quando meu 3,4,5-TMOBA chegar.
Aprendi quando fiz a reação de nitro também com o 2,5-DMOBA que vale a pena, em termos de quantidade de nitroalcano, ter o catalisador correto!

Alguém sabe se eu poderia usar a ciclohexilamina como catalisador para a reação de Henry do 3,4,5-TMOBA usando nitroetano, para que eu possa reduzir ao TMA correspondente, bem como ao intermediário b-nitrostyrene para a mescalina?

 

[handle]

No freezer agora. Atualizarei com os resultados em breve. Minha mistura sempre fica com uma cor vermelho-escura, não fica amarelo-claro. É possível que o benzaldeído seja de baixa pureza? Ou superaquecimento? Ou ambos?

 

[handle]

Não estou satisfeito com esse resultado.

 

[BevItUp]

Não sei @handle, acho que seu resultado final ficou muito bom. Não é exatamente o mesmo amarelo, mas eu diria que está dentro da faixa de desvio normal.
A única coisa que eu estava observando era a cristalização. Na foto, eles parecem pequenos quadrados e não têm a aparência de fibra de vidro. Mas ei... feito em casa usando um micro-ondas??? Parece muito bom.

Além disso, as duas primeiras parecem com a cerveja caseira do meu sogro alemão

 

[handle]

Sim, o rendimento foi horrível! 10 g de 80 ml de NE + 80 ml de B + 20 ml de GAA + 18 ml de A
Tenho quase certeza de que superaqueci o RM na terceira radiação, pois ele ferveu e passou da cor mais clara para aquela "cor escura de alcatrão".
Não ajudou o fato de o micro-ondas estar em 1100W....
Primeiro tentei 70% por 1 minuto a 770 W, mas foi muito longo e muito quente.
A radiação seguinte foi de 60% por 30 segundos a 660 W, que foi muito curta e muito fria.
A terceira radiação foi de 60% por 1 minuto a 660 W, o que foi um pouco longo demais.
45 segundos a 660 W foi o ideal, mas aí já era tarde demais. É importante manter o RM em 60 °C ou um pouco abaixo
Da próxima vez, já sei que vou começar com 60% por 45 segundos a 660 W, ahhh ciência.

 

[rampage]

hey bro
did you need to tape the rubber glove to the beaker?

 

[Osmosis Vanderwaal]

When I was reading about microwave reactions 10 years ago and based on what it said, you have to do a little wiring to get goodmresults. Most microwaves use a duty cycle to adjust the heat, so if you put it on 40% , youndont get 40% power, you get 100% for 40% of a cycle. Also it said laboratory microwaves operatednat a lower frequency, which i havent looked into but it should be easy to change ( or gut and use a sinewave generator so its adjustable)

 

[rampage]

my old microwave is 500w as low and 600w as high. its got the old turn a nob for power level and for irradiation time, so each time i started it i also started a stop watch and when i see a bubble boil i quickly stopped the microwave and the stop watch and this is how i got my irradiation times, different irradiation times are probably going to be acheived depending on temp of rm before irradiation also volume of rm and whatever power settings one goes with, just remember to stop it when you see those first 1 or 2 bubbles boil to the surface. try and keep the glove on the hole time, swirl it when kooling and gently dunk into a water bath when kool enough to speed up the process of bringing it back to room temp, even the magnetic stirrer could be implemented after each irradiation while the rm is kooling.

 

[rampage]

does anyone know if you need to tape the rubber glove to the beaker?

 

[rampage]

do not tape rubber glove!!! just choose a glove size that fits tightly on beacker.

 

[rampage]

okay finished attempt 1 and attempt 2
microwave synth of p2np

50ml nitroethane, 13ml of gaa, 20ml of n-butylamine and 50ml of benzaldehyde, mixed in that order.
allow mixture to sit for 5 minutes as the rm comes together and smoke vapour clears.
place a rubber dishwashing glove onto beaker, i used the cheapest one available at supermarket.

microwave is 500 to 600w, 600w is the high setting and 500w is the low setting, i use in this synth, the settings high = 600w and med/high = 575w.

place rm into the microwave.
1st irradiation was 40 seconds on high, removed rm and cooled to room temp

2nd irradiation was 45 sec on med/high, removed rm and cooled to room temp

3rd irradiation was 50 sec on med/high, removed rm and cooled to room temp


4th irradiation was 1 minute on med/high, removed rm and cooled to room temp

5th irradiation was 1 minute on med/high, removed rm and cooled to room temp

6th irradiation was 1 minute on med/high, removed rm and cooled to room temp

7th irradiation was 1.10 min/sec on med/high, removed and cooled to room temp


200mls of 100% ipa was added to the rm, then covered with glad wrap and placed in the freezer.
i took a little bit of the reaction mixture and evaporated to get a seed crystal.

once i added the seed crystal, boom p2np instantly crystallized.

i then placed rm back in the freezer.
i will vacuum filter shortly and wash crystals with amount of cold ipa, then weigh crystals.

then will place motherliquour back in freezer for a second crop.


attempt 2 i did straight after attempt 1

place
100ml of nitroethane
25ml of gaa
20ml of n-butylamine - towards the end of the reaction i notice unreacted benz so i add another 10ml of n-butylamine so n-butylamine = 30mls!
100ml of benzaldehyde
in to a beaker and allow rm to react for 5 minutes, clear smoke and place rubber glove onto beaker.

place into microwave,

1st irradiation was 1.50 min/sec on med/high, removed rm and cooled to room temp

2nd irradiation was 1.20 min/sec on med/high, removed rm and cooled to room temp

3rd irradiation was 1.40 min/sec on med/high, removed rm and cooled to room temp

4th irradiation was 1.30 min/sec on med/high, removed rm and cooled to room temp

5th irradiation was 1 minute on high, removed rm and cooled to room temp

6th irradiation was 1.25 min/sec on high, removed rm and placed a magnetic stir bar into the beacker and stirred for 20 minutes as rm cooled to room temp

7th irradiation was 1.10 min/sec on high, removed rm and stirred for 30 minutes as rm cooled to room temp.

added seed crystal and boom p2np instantly crystallizers,









placed in freezer and will vacuum distill shortly and wash with cold ipa.

this photo is both attempts....

i will publish the weights soon...

 

[Osmosis Vanderwaal]

Isnthere any sort of theme to your times, that you are irradiating it for? Does it boil? I guess not since the glove doesnt melt. What is the polar chemical heating the solution?

 

[rampage]

yeah, cause i did it at night i used a torch to see thru the door on the microwave and as soon as there was 1 or 2 boiling bubbles i stopped the microwave, it was really only the first irradiation that was a concern, as soon as it started to boil it was stopped but the reaction kept going for a good couple of minutes by itself, this is why not to tape the glove as the reaction ballooned it too almost coming off, where the rest of the irradiations it doesnt react violently after its stopped as long as you stopp it when 1 or 2 bubbles boil to the surface, the 50ml attempt was reasonably straight forward the rm seemed to be as 1 the whole way thru, the 100ml attempt was a different scenario it sorta layered itself whenever it settled and by the 5th irradiation there seemed to be an oily unreacted benzaldehyde layer on the bottom,so there was 3 layers, so i added another 10ml of n-butylamine and chucked in a stir bar and put it on the magnetic stirrer for 20mins then did the next irradiation and then back on the stirrer for 30mins and this seemed to bring it back to two layers, thin layer on top and the bottom layer as 1, cooled to room temp added ipa, found that adding pretty much 1:1 ipa to rm volume or even a little bit more aloud for a greater crop of crystal as soon as it was seeded, crystallization happened very quickly. i even got the second crop very quickly after adding water to the motherliquor and putting it back in the freezer, the recovered p2np is still drying to dry weight and i should have the final weights very soon and i will post them when i do probably in a couple of hrs. this is my first attempts at this and it seemed to all go to plan, so i'm pretty happy at the moment. i irradiated it between 575watts and 600watts and found it to be okay. if there's anymore questions i'm happy to answer them this is a very user friendly synth and im expecting good yields.

 

[rampage]

attempt number 1, 50ml synth, yield = 63 gms dry weight
attempt number 2, 100ml synth, yield = 137gms dry weight
combined second pull = 15gms dry weight

combined weight = 215gms dry weight of p2np

 

[Osmosis Vanderwaal]

Methanol ( probaby among other things) is polar, which is a prerequisite to microwave irradiationmas far as I know, its what the microwaves vibrate whichcauses the heating effect, if i understand correctly. Thisnisnvery interesting to me but at the same time all of theose chemicals are a pain to get very much of. Did you use technical grade benzaldehyde or is it immitation vanilla/ almond?

 

[rampage]

yeah benzaldehyde is pure not an immitation. nitroethane 100%