Need help with P2P Synthesis - Sodium Cyanide

[Needtolearn]

Hi i first of let me thank the people who made this forum and keeping knowledge alive in the world. i have spent the past few years seeking a way to make P2P from scratch i have come up with this list and recipe. My main issue is thet i live in a country where Toothpaste, soap and detergents is basicly all chemicals that is legal to have. so for me it seems like a total Synthesis is the only route i can take.

From all my readings i will be able to collect/make all the chemicals in this list. but when i prepared the Sodium Cyanide it was no where near the purity needed to react with benzyl chloride. i did follow follow Nurdrage`s method =

So my question is how can i make pure (98%) Sodium Cyanide or purification of crude sodium cyanide from video above to make Benzylcyanide ? or even better is there a way where i can not make cyanide at all. i absolutely hate the fact that i will be working with it.

Any one here that sees this list wil also ounderstand it is a substanstial amount of chemicals to make 1.3 kg P2P that - will be used to make 1 kg Amphetamine Sulfate. the problem for me now is that this will bring the total cost for me in my country arround 3200 USD (for the P2P) and 1200 USD to convert P2P to Amphetamine Sulfate. (4400 USD/Kg)

Any advise to cut cost and maby shorter paths will be mutch appritiated. the "recipe" and list of chemicals is listed below

Phenyl-2-Propanone from Benzyl Cyanide​

​

alpha-Phenylacetoacetonitrile



A solution of sodium ethoxide is prepared from 60 g. (2.6 mol) Clean Sodium and

700 ml of 100% Alcohol (dried over calcium oxide or sodium) in a 2000 ml round-bottomed flask equipped with a reflux condenser. To the hot solution added a mixture of

234g (2 moles) of pure Benzyl Cyanide «C₆H₅CH2CN» and

264g (3 moles) of dry Ethyl Acetate «CH₃CH₂OCCH₃» (dried by refluxing for 30 min over P2O5 followed by distillation). The mixture is thoroughly shaken, the condenser closed with a Calcium Chloride tube, and the solution heated on the steam bath for two hours before standing overnight.


The next morning the mixture is stirred with a wooden rod to break lumps, cooled in a freezing mixture to -10°C, and kept at this temperature for two hours.


The sodium salt is collected on a 6-inch Buchner funnel and washed four times on the funnel with 250 ml portions of Ether. The filter cake is practically colourless and corresponds 250-275g of dry sodium salt, or 69-76% of the calculated mount.


The combined filtrates are placed in the freezing mixture until they can be worked up as indicated below.


The sodium salt still wet with ether is dissolved in 1.3 litres of Distilled Water at room temperature, the solution cooled to 0°C, and the nitrile precipitated by adding slowly, with vigorous shaking, 90 ml of Glacial Acetic Acid, while the temperature is kept below 10°C.



The precipitate separated by suction filtration and washed four times on the funnel with 250 ml portions of water. The moist cake weighing about 300g corresponds to 188-206g (59-64%) of dry colorless alpha-phenylacetoacetonitrile, mp 87-89°C.


Phenyl-2-Propanone


350 ml of concentrated sulfuric acid is placed in a 3000ml flask and cooled to -10°C. The total first crop of moist alpha-phenylacetoacetonitrile obtained according to the procedure above (corresponding to 188-206g or 1.2-1.3 moles of dry product)


is added slowly, with shaking, the temp being kept below 20°C (If pure dry alpha-phenylacetoacetonitrile is used, half its weight of water should be added to the sulfuric acid or charring will take place on the steam bath).


After all is added the flask is warmed on the steam bath until solution is complete and then for five minutes longer.


The solution is cooled to 0°C, 1750ml of water added rapidly, and the flask placed on a vigorously boiling water bath and heated for two hours, with occasional shaking.


The ketone forms a layer and, after cooling, is separated and the acid layer extracted with 600ml of Ether. The oil and ether layers are washed successively with

100ml of water, the ether combined with the oil and dried over 20g of anhydrous Sodium Sulfate. The sodium sulfate is collected on a filter, washed with Ether, and discarded. The ether is removed from the filtrates, and the residue distilled from a modified Claisen flask with a 25 cm fractionating side arm.

The fraction boiling at 110-112°C at 24 mmHg is collected; it weighs 125-150g (77-86% of the theoretical amount).

Natrium metall (1)
Mengde	Norsk Navn	Engelsk navn	Formel
1600g	Natriumhydroksid	Sodium Hydroxide	NaOH
500g	Magnesium metall	Magnesium	MG
1L	Dioksan	Dioxane	C4H8O2
	=600g Natrium metal	= 600g Sodium Metal
Natriumcyanid (NaCN) Sodium cyanide 98 % (2)​
8800g	Natriumhydroksid	Sodium Hydroxide	NaOH
3520g	Urea	Ureea	CON₂H₄
960g	Karbon	Carbon	C
10 L	Metanol	Methanol	CH3OH
8480g	Natriumbikarbonat	Sodium Bicarbonate	NaHCO₃
	=1,6 kg Natrium cyanid	=1,6 kg Sodium cyanid
Benzylklorid (C3H3CH2CI) - Benzyl chloride (3)​
2300g	Natriumhydroksid	Sodium Hydroxide	NaOH
3400g	Tørr Toluen	Toluene	C7H8
	=3125g Benzylklorid	= 3125g Benzyl Chloride
Benzylcyanid (C6H5CH2CN) – Benzylcyanide (4)​
1600g	Natriumcyanid 98 % (2)	Sodium Cyanide	NaCN
3125g	Benzylklorid (3)	Benzyl Chloride	C6H5CH2Cl
900ml	Destillert Vann	Destilled Water	H2O
3,5L	Etanol 100% (Sprit)	Ethanol	C2H5OH
	= 2343g Benzylcyanide	= 2343g Benzylcyanide
Tørr Etylacetat (CH₃CH₂OCCH₃) Anhydrous ethyl acetate (5)​
2,9L	Etylacetat	Ethyl Acetate	CH₃CH₂OCCH
260g	Fosforpentoksid	Phosphorus Pentoxide	P2O5
	=2,7L Tørr Etylacetat	= 2,7L Anhydrous ethyl acetate
Iseddik ( CH₃COOH ) Glacial Acetic Acid (6)​
1,3kg	Natriumacetat	Sodium Acetate	C2H3NaO2
1950ml	Svovel Syre	Sulfuric Acid	H2SO4
	=900ml iseddik	= 900ml Glacial Acetic Acid
P2P- Fenylaceton (C6H5CH2COCH3) – Phenylacetone​
600g (26mol)	Natrium metal (1)	Sodium Metal	NA
7L	Etanol 100% (Sprit)	Ethanol	C2H5OH
1,5kg	Kalsiumklorid (7)​	Calcium Chloride	CaCl2
2,4L (20mol)	Benzylcyanide (2,3,4)​	Benzylcyanid	C6H5CH2CN
2,7L (30mol)	Tørr Etylacetat (5)	Ethyl Acetate	CH₃CH₂OCCH
8L D vann	Destillert Vann	Destilled Water	H2O
6L	Diethyl Ether (8)	Diethyl Ether	(C2H5)2O
500g	Natriumsulfat (9)​	Sodium Sulfate	Na2SO4
900ml	Iseddik (6)	Glacial Acetic Acid​	CH₃COOH
3,5L	Svovel Syre (10)	Sulfuric Acid	H2SO4
	= 1300g Fenylaceton	​	C₆H₅CH₂COCH₃

 

[G.Patton]

Have you thought about P2P synthesis via Grignard reagent? https://chemforum.info/index.php?threads/phenylacetone-p2p-syntheses-via-grignard-reagents.636/
You can make toluene from benzene and after, make benzene chloride. Or oxidize toluene to benzaldehyde.

 

[G.Patton]

To further purify NaCN, there are two ways:​

• The safe, slow way: convert the impure NaCN into Prussian blue, filter it from the solution, calcinate the Prussian blue using molten sodium hydroxide to reconvert it back into NaCN, and purify it by recrystallizing it from ethanol and water.​
• The dangerous, quick way: convert the NaCN into Prussian blue, then add conc. sulfuric acid and gently heat the flask to distill the resulting HCN and bubble it in a cooled alcoholic solution of NaOH (methanol is a good choice). Since this route involves working with gaseous HCN, do not do this unless you have experience and this absolutely must be done outside or under a fumehood. Impure NaCN tends to have some sodium cyanate which in contact with a strong acid releases isocyanic acid, which may contaminate your distillate, but also has lots of sodium carbonate, which will release carbon dioxide upon reaction with an acid, which will react with your sodium hydroxide and form sodium carbonate again, contaminating your final product.​

 

[Needtolearn]

Thank you so much. I apologize in advance for beeing somewhat retarded and asking many questions. but there is just so many possible routes to take but all of them contains at least one or more chemicals that is nearly impossible to get. But I would love to try the Grignard regent but i am unable to get Dry ice when this is a controlled substance in my country. i can buy dry ice for "sand" blasting (tiny pellets of solid Co2) but its a little expensive and last i checked minimum order is somthing stupid like 600kg/order. this would be no problem when i have sorted material list and perfected the syntesis and are ready to start production.

How would one oxidize toluene to make benzeldehyde? if this method is some what high yielding? then i can make P2NP and use it instead. But it is still somewhat painfull to make nitroethane Sodium nitrate is impossible to buy (i can buy meat aging salt with 3% nitrate inside) but this is also stupidly expensive and as far as i know it would be impossible to separate the salts? that means unless i can make apparatus and make my own my, only option to obtain it will be to smuggle it from another country witch means i could just smuggle the finished product instead.

"The safe, slow way: convert the impure NaCN into Prussian blue, filter it from the solution, calcinate the Prussian blue using molten sodium hydroxide to reconvert it back into NaCN, and purify it by recrystallizing it from ethanol and water."

I found this one online. i do not understand how that will work. and if this method works - would it not be easyer/ make more sense to buy prussian blue from a comapny? as far as i know this is a textile dye so it should not be a limited chemical? any one here know if prussian blue is on any watch lists?

 

[G.Patton]

any one here know if prussian blue is on any watch lists?

NeedtolearnHello, I don't think so.

i do not understand how that will work.

The release is not violent at all. The cyanide ligands are attached to the iron cores very tightly. If you want to release HCN from this compound, then you need to add it to dilute sulphuric acid (30% or so) and heat. In that case, HCN is released, but even then, is it going slowly. A high concentration of phosphoric acid most likely will release HCN as well, but this also will require heating.

Bubbling the HCN through an aqueous solution of NaOH or KOH does not give you the cyanide when the solution is evaporated to dryness. Much of the HCN is released again under such conditions, and at best you get a highly alkaline NaCN/NaOH mix. There also will be side reactions, in which HCN/CN(-) is oxidized and you most likely get brown crap.

You could try getting NaCN from ethanol or methanol solution of NaOH.

Beware, working with HCN is EXTREMELY dangerous. Something like 50 mg of the gas can knock you down! If you don't have extensive experience with complex chemical apparatus, then DON'T MAKE HCN as you suggested.

Keep an antidote kit nearby (amyl nitrate, IIRC sodium thiosulfate with some nitrite also works) and never work alone with HCN. Also, be sure how to apply the antidote if necessary. Study this before doing any work with HCN, both you and the other person, who is nearby.

 

[Needtolearn]

Thank you for answer. i do use pressurized breathing system with positive pressured suit. and the reaction "box/room" is also in negative pressure with a stupid redundant airflow that leads to a filtration system. but i have been looking at other ways to do the synthesis to reduce need for chemicals right now the volume needed to produce 1 kg is way to high. lowest current calculated weight of all chemicals including acids i am now at 67kg to make 1 kg amphetamine.