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
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).
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-PhenylacetoacetonitrileA 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 |
