Mikrobangų krosnelės (mažos) apimties: 1-fenil-2-nitropropenas (P2NP)

[handle]

Ar kas nors pastaruoju metu išbandė būtent šį receptą? Žinau, kad Jesse_pinkman_ tai darė prieš kelerius metus. Bet tada jis išėjo į galą...

Norėtųsi išgirsti kokių nors patirčių, pamokymų, patarimų, patobulinimų ar gudrybių? Ačiū visiems iš anksto.

Mikrobangų krosnelės (maža) skalė:
1. Benzaldehidas 100 ml, nitroetanas 100 ml, ledinė acto rūgštis 25 ml ir n-butilaminas 20 ml supilami į 500 ml stiklinę.
2. Ant ąsočio uždedama guminė pirštinė.
3. Ąsotis įdedamas į mikrobangų krosnelę.
4. Mikrobangų krosnelės galia nustatoma 750 W. Krosnelė įjungiama ir mišinys šildomas, kol užverda. Mišinys atvėsinamas iki kambario temperatūros.
5. 4 veiksmas kartojamas kelis kartus. Mažiausiai 6 kartus.
6. Po to įpilama 100 ml IPA, reakcijos mišinys išmaišomas ir 12 valandų dedamas į šaldiklį. 1-fenil-2-nitropropenas(P2NP) susikristalizuoja.
7. Produktas P2NP filtruojamas Buchnerio piltuvu(siurbimo filtravimo procedūra), nuplaunamas nedideliu kiekiu šalto IPA ir džiovinamas ore (arba vakuuminėje kameroje, pasirinktinai).

 

[HIGGS BOSSON]

Šiuo metodu mikrobangų krosnelėje gaminau nedidelius kiekius (iki 100 g), viskas gaunasi gana paprastai.

 

[handle]

25 ml GAA į 20 ml amino, ar tai geriausia? Mano skaičiuotuvas nurodė, kad 40ml GAA ir 20ml amino. Laikysiuosi 25ml, nebent man patartų kitaip.

 

[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]

ketinu tai išbandyti, kai tik bus atsargų

 

[Rabidreject]

Reikalas tas, kad manau, jog geriau pasiliksiu nitroetaną tam atvejui, kai ateis mano 3,4,5-TMOBA, o aš nenoriu p2np pakankamai stipriai, kad vargčiau gaudamas n-butilaminą....bet girdėjau, kad kiti stambūs aminai taip pat tinka... ar tiktų trietilaminas?

 

[Rabidreject]

Ooo tai įdomu...

Iš tikrųjų planuoju pabandyti pasigaminti cikloheksilamino...

Ketinau pabandyti sukurti vaizdo įrašą apie tai, nes "YouTube" nėra nė vieno vaizdo įrašo - mane tai nustebino... jei iš tikrųjų pavyks jį paleisti, tai yra, lol

Mes pamatysime, bet jei ne, aš galiu tiesiog nusipirkti jį, kai mano 3,4,5-TMOBA ateina.
Atlikdamas nitro reakciją su 2,5-DMOBA sužinojau, kad teisingas katalizatorius atsiperka nitroalkano kiekio prasme!

Ar kas nors žino, ar galėčiau naudoti cikloheksilaminą kaip katalizatorių Henrio reakcijai su 3,4,5-TMOBA naudojant nitroetaną, kad galėčiau redukuoti iki atitinkamo TMA, taip pat b-nitrostireno tarpinio junginio meskalinui?

 

[handle]

Dabar šaldiklyje. Netrukus atnaujinsiu su rezultatais. Mano mišinys visada tampa tamsiai raudonos spalvos, neišlieka šviesiai geltonas. Galbūt benzaldehidas yra mažesnio grynumo? Arba perkaitimas? Arba ir viena, ir kita?

 

[handle]

Nepatenkinti šiuo rezultatu.

 

[BevItUp]

Nežinau, @handle, manau, kad jūsų galutinis rezultatas atrodo gana gerai. Jis nėra lygiai tokios pat geltonos spalvos, bet sakyčiau, kad tai normalaus nuokrypio ribose.
Vienintelis dalykas, į kurį savotiškai žiūrėjau, buvo kristalizacija. Nuotraukoje jie atrodo kaip maži kvadratėliai ir neturi stiklo pluošto išvaizdos. Bet ei... naminė naudojant mikrobangų krosnelę???? Atrodo gana gerai.

Be to, pirmoji pora atrodo kaip mano vokiškojo uošvio naminis alus

 

[handle]

Taip, jų išeiga buvo siaubinga ! 10 g. iš 80 ml NE + 80 ml B + 20 ml GAA + 18 ml A
Esu beveik tikras, kad perkaitinau RM per trečiąjį spinduliavimą, nes jis užvirė ir iš šviesios spalvos tapo tos "tamsios poli deguto spalvos".
Nepadėjo ir tai, kad mikrobangų krosnelė buvo 1100W....
Pirmiausia bandžiau 70 % 1 minutę @ 770 W, tai buvo per ilgai ir per karšta.
Kitą kartą spinduliavimą atlikau 60 % 30 s @ 660 W, kuris buvo per trumpas ir per šaltas.
Trečiasis spinduliavimas buvo 60 % 1 minutę @ 660 W, tai buvo šiek tiek per ilgai.
45 sekundės @ 660 W buvo tinkamos, bet tada jau buvo per vėlu, svarbu, kad RM būtų 60 °C arba šiek tiek mažesnė.
Kitą kartą žinau, kad reikia pradėti nuo 60 % 45 sekundes @ 660 W, ahhhhh mokslas.

 

[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%