Mikrohullámú (kis) lépték: 1-fenil-2-nitropropén (P2NP)

[handle]

Próbálta valaki mostanában ezt a pontos receptet? Tudom, hogy Jesse_pinkman_ néhány évvel ezelőtt megtette. De aztán elment egy Gallium érintőlegesen...

Szeretnék hallani néhány tapasztalatot, tanulságokat, tippeket, finomításokat vagy trükköket? Köszönöm mindenkinek előre is.

Mikrohullámú (kis) skála:
1. Benzaldehid 100 ml, nitroetán 100 ml, jégecetsav 25 ml és n-butilamin 20 ml kerül 500 ml-es főzőpohárba.
2. A főzőpohárra gumikesztyűt húzunk.
3. A főzőpoharat mikrohullámú sütőbe tesszük.
4. A mikrohullámú sütő teljesítményét 750 W-ra állítjuk. A sütőt bekapcsoljuk, és a keveréket forrásig melegítjük. A keveréket szobahőmérsékletre hűtjük.
5. A 4. lépést többször megismételjük. Minimum 6 alkalommal.
6. Ezután 100 ml IPA-t adunk hozzá, a reakcióelegyet megkeverjük, és 12 órára fagyasztóba tesszük. Az 1-fenil-2-nitropropént(P2NP) kikristályosítjuk.
7. A P2NP terméket Buchner-tölcséren szűrjük(szívószűrési eljárás), kis mennyiségű hideg IPA-val mossuk és levegőn (vagy vákuumkamrában, opcionálisan) szárítjuk.

 

[HIGGS BOSSON]

Kis mennyiségeket (100g-ig) készítettem mikrohullámú sütőben ezzel a módszerrel, minden nagyon egyszerűen kiderül.

 

[handle]

A 25ml GAA 20ml aminhoz a legjobb? A számológépem azt mondta, hogy 40ml GAA 20ml aminhoz. Én maradok a 25ml-nél, hacsak nem tanácsolnak mást.

 

[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]

Megpróbálom ezt, amint a készletek itt vannak

 

[Rabidreject]

Az a helyzet, hogy szerintem inkább tartogatom a nitroetánt arra az esetre, ha jön a 3,4,5-TMOBA, és nem akarok p2np-t annyira, hogy n-butilamin beszerzésével bajlódjak....de iv hallottam, hogy más terjedelmes aminok is működnek... trietilamin is működne?

 

[Rabidreject]

Ooo ez érdekes...

Valójában azt tervezem, hogy megpróbálok egy kis ciklohexilamint készíteni...

Meg akartam próbálni egy videót készíteni róla, mivel nincs egy sem a YouTube-on - ez meglepett engem... ha tényleg sikerül rávenni, hogy működjön, akkor lol

Meglátjuk, de ha nem, akkor csak akkor vásárolhatom meg, amikor az én 3,4,5-TMOBA jön.
Megtanultam, amikor a 2,5-DMOBA-n a nitro is reakciót csináltam, hogy a nitroalkán mennyisége szempontjából kifizetődő a megfelelő katalizátor!

Tudja valaki, hogy a 3,4,5-TMOBA Henry-reakciójához nitroetán felhasználásával ciklohexilamint használhatnék-e katalizátorként, hogy a megfelelő TMA-ra, valamint a meszkalin b-nitrosztirén köztitermékre redukálhassam?

 

[handle]

Most a fagyasztóban. Hamarosan frissítjük az eredményekkel. A keverékem mindig sötétvörös színűvé válik, nem marad világossárga. Lehetséges, hogy a benzaldehid kisebb tisztaságú? Vagy túlmelegedett? Vagy mindkettő?

 

[handle]

Nem elégedett az eredménnyel.

 

[BevItUp]

Nem tudom @handle, szerintem a végeredményed elég jól néz ki. Nem pontosan ugyanolyan sárga, de azt mondanám, hogy a normális eltérésen belül van.
Az egyetlen dolog, amit valahogy néztem, az a kristályosodás. A képen kis négyzeteknek tűnnek, és nem olyan üvegszálasak. De hé... házi készítésű mikrohullámú sütővel???? Elég jónak tűnik.

Az első pár úgy néz ki, mint a német apósom házi készítésű söre...

 

[handle]

Igen, a hozamuk borzalmas volt ! 10 g. 80 ml NE + 80 ml B + 20 ml GAA + 18 ml A
Elég biztos, hogy túlmelegítettem az RM-et a harmadik sugárzásnál, mivel felforrt és a világosabb színből a "sötét poli kátrányos színűvé" vált.
Nem segített, hogy a mikrohullámú sütő 1100W.... volt.
Először megpróbáltam 70%-os 1 percig 770W-on, ez túl hosszú volt és túl forró.
A következő sugárzást 60%-on csináltam 30 másodpercig 660W-on, ami túl rövid és túl hideg volt.
A 3. sugárzás 60% volt 1 percig 660W-on, ez egy kicsit túl hosszú volt.
A 45 másodperc 660W-on nagyjából megfelelő volt, de akkor már túl késő volt, fontos, hogy az RM-et 60c-on vagy valamivel 60c alatt tartsuk.
Legközelebb már tudom, hogy 60%-on kezdem 45 másodpercig 660W-on, ahhh tudomány.

 

[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%