# BMK (benzylmethylketone) synthesis from APAAN (a-phenylacetoacetonitrile). Large scale.



## William Dampier

​*APAAN* is frequently used for BMK (P2P; cas 103-79-7) production by following reasons:
• The APAAN (cas 4468-48-8) price of is relatively low in compare with P2P price;
• APAAN conversion to BMK doesn't require specific chemistry knowledge;
• APAAN conversion to BMK doesn't require complex or expensive equipment;
• A good enough yield 60-75% is easily achieved.

APAAN can be converted with help of a strong acid such as phosphoric acid, sulphuric acid or hydrochloric acid. An external heating is also needed to some reaction ways. Synthesis products are BMK (P2P), ammonium salt, CO2, some remaining acid and water.​

​APAAN conversion product mixture usually contains mixture of BMK, acid, water, ammonium salt, and APAAN sometimes (depends on substances ratios). It is happen by reason that this synthesis is usually carried out at bad laboratory conditions with some mistakes. In addition, the product mixture contains a by-product row, which are synthesized from BMK in acidic space.

According with public information, a number of chemists use an excess of acids in order to increase conversion speed and carry out complete APAAN conversion to BMK. Acidic water layer will be in final product mixture in case of aqueous acid solution using. It looks like two layers, oily top layer is BMK, acidic water layer is bottom one.

APAAN conversion of BMK is carried out in several stages:​

​APAAN to BMK conversion is a hydrolysis reaction. This is a reaction with water that can be carried out using an acid (hydrochloric acid, sulphuric acid or phosphoric acid) or a strong base, such as caustic soda (sodium hydroxide).

The reaction has several stages. For example, -CN group is converted into acid group -COOH in hydrochloric acid reaction condition, then ammonium chloride is formed. Ammonium chloride is NH4CL, which contains the N atom of the -CN group. If sulphuric acid is used in the reaction, ammonium sulphate is formed in this stage.

Decarboxylation takes place in the following reaction stage. This means that CO2 is formed out from acid group. After this, the APAAN conversion to BMK is completed. HCN is extremely poisonous hydrocyanic acid, formed during the reaction at normal conditions. It is unknown what happens, if the same reaction takes place at very high temperature. This can happen only in case, if there is no water remains in the reaction system. The reaction mixture boiling point is 100 °C because there is water. APAAN has liquid form at 100°C, which make mixing process simple.​
*APAAN conversion with phosphoric acid*



​
*Description of the chemical procedure:*
APAAN is mixed with phosphoric acid in the first stage. Then, the mixture have to be heated to 150 - 160 °C for proper conversion. This is a much higher temperature then in reactions with sulphuric acid or hydrochloric acid. Water isn't added to the reaction mixture. Water prevents the temperature reaching the high temperature by reason that water b.p. is 100 °C.

The mixture is heated for several hours. The oily crude top BMK layer is separated from the acidic bottom layer. The bottom layer consists of acid with some BMK remains, ammonium phosphate and some unconverted APAAN.​
*Description of the technical process:*
The reaction takes external heating by reason that the reaction mixture need to reach 150-160 °C with phosphoric acid hydrolysis. There are several options such as electric heating mantles and gas burners, which have the disadvantage that exact temperature control is impossible. Also, electric heating in combination with silicone oil is available.​

​Glass vessels such as round bottom flasks or reaction flasks can be used as reaction vessels. Metal reaction vessels with a protective coating such as enamel or Teflon on the inside can also be used (not recommended). The coating maintains metal vessel from strong acids to avoid a corrosion.​

​
*APAAN conversion with sulphuric acid*



​
Two synthesis ways with sulphuric acid were found:

*a.* A way with external heating source application;
*b.* A self-heating by an exothermic reaction between sulphuric acid and water;
*External heating source application*
This conversion method takes a heating source. In the first APAAN conversion labs that were found, 22 L preserving kettles were frequently used. An advantage of these kettles is that they can be easily modified. It is simple to make holes in order to install exhaust pipes for fumes, gases and a stirring mechanism.​
*The chemical process description*
Stage 1: APAAN is mixed with water and concentrated sulphuric acid. The sulphuric acid may be slightly diluted beforehand. The mixture have to be cooled by reason that the mixing process generates a lot of warm. The reaction mixture can be cooled to 100 °C, which makes it possible to immediately proceed to stage 2.

Stage 2: The mixture is kept at 100 °C for a while and then cooled to room temperature.​

​Stage 3: A large water volume is added to the mixture. Then, it is cooled to a correct temperature.

Stage 4: The reaction mixture is heated to 100 °C and kept at this temperature for several hours. Oily crude BMK (P2P) is separated from the acidic bottom aqueous layer during this procedure. The bottom layer consists of diluted sulphuric acid with dissolved BMK, ammonium sulphate, unconverted APAAN traces and by-products.​
The mixture ratio: APAAN 2.2 kg, concentrated sulphuric acid (H2SO4) 4 L and water 12 L. 

*Description of the technical process:*
APAAN is mixed with concentrated sulphuric acid in the first production stage. The heat, which is generated during this process, have to be reduced by cooling. A cooling system, which is consist of a mortar tub with a drainage pipe in the base, was installed when preserving kettles were used. The preserving kettle is placed on three bricks on the tub bottom. Bricks have prevented the preserving kettle from touching the wet tub base and the electric heating element from continued exposure by water.

A ring of plastic tubing equipped with thin nozzles inside, is installed on a top of the mortar tub. This tubing is attached to the water pipes, so that nozzles are sprayed cold water against the outside of the preserving kettle. It allows to reduce the reaction mixture temperature gradually. Similar cooling system is shown. A ring of tubing around the reaction vessel is described in other conversion methods.​

​A 24 Volt electric motor is located on preserving kettles top, which runs a stirring mechanism. APAAN with an acid are mixed during the reaction.

The mixture is transferred to a second set of processing equipment after completion of the second stage. Preserving kettles without a cooling system have been used in this case. Water is added after the mixture has been transferred. The mixture is then heated to a temperature of 95 - 100 °C. Several preserving kettles are used simultaneously by reason that a production capacity is limited about 1.5 to 2 litres of BMK per one production batch. All of them are attached to an exhaust system that removes the poisonous or harmful fumes and gases.​


​
*The exothermic reaction self-heating by sulphuric acid and water*
This conversion method doesn't use an external heating source. A reaction heating, which is generated by sulphuric acid with water reaction, is used. The rate, at which water is added, is determined by an amount of a generated heating.​
*Description of the chemical process:*
Stage 1: APAAN is mixed with water and concentrated sulphuric acid. A heating is generated, during this reaction, the mixture must be cooled.

Stage 2: A large quantity of water is added to the mixture after cooling. It must be done in a controlled way. The reaction between water and sulphuric acid generates a great amount of heat, which should be limited by addition of cold water in portions over several hours. The temperature should not be risen too much. The oily crude BMK (P2P) is separated from the acidic bottom layer during this process. The bottom layer consists of diluted sulphuric acid, small amount of BMK, ammonium sulphate, unconverted APAAN traces and a some by-products.​
*Description of the technical process:*
This conversion method is similar to the method, which uses an external heat source. The first laboratory, where this method was used, was found in Feb 2011. A plastic reaction vessel 750 L was used in this lab.

This reaction vessel was equipped with a cooling system on the outside as in the preserving kettles method. This system consists of a copper pipes ring with nozzles. The metal pipe system had been sealed with foil that was caught the cooling water outside. Warm water was added with help of a pump to heat the reaction mixture. The reaction temperature was controlled by an electronic thermometer during conversion process.​

​The vessel content was stirred with a stirrer mechanism. Fumes and gases, which was released during the process, were cooled with help of a cooling system. It was made from double-walled PVC tubes. This cooling system could be equipped with active carbon filters at the pipe end.

A large-scale conversion set-up like this was found only once. Usually, plastic barrels with band clamp lids are used, which are placed in a mortar tub. A similar cooling system is installed around the lids of these barrels. The mixture is stirred by an electrically powered stirring mechanism installed over the barrel. A disadvantage of this conversion set-up is that, unlike the preserving kettles and the plastic vessels mentioned above, this is an open process, which means that fumes and gases are released from the open-top of the barrel and will spread freely throughout the production space. Therefore, the air in the production space should be extracted by an exhaust system, possibly in combination with an active carbon filter.

The emission from the reaction vessel into the production space is a major disadvantage of this set-up. Illegal producers, as well as investigation and emergency services, will be exposed to these fumes and gases in the case of a calamity and/or investigation. In addition, the material in the production space will be contaminated and corroded by the acid and poisonous fumes and gases. Further, processing of the content of such large set-ups was shown to cause considerable pollution of the location.​

​
*APAAN conversion with hydrochloric acid*​

​Stage 1 – The conversion reaction
APAAN is mixed with hydrochloric acid, at a ratio of APAAN 1 L to hydrochloric acid 3 L 36%. This mixture must be stirred thoroughly, and heated to 95 °C for 10 hours with a constant stirring. The fumes and gases, which is generated during the process, are removed through a gas scrubber, which neutralizes them.

The heaters are turned off as soon as the conversion reaction is complete. The acidic, dark brown BMK will float on top of the fluid. It can be separated using a separatory funnel. If large quantities of APAAN have been converted into BMK, the BMK can be skimmed off using a metal ladle.​
*Description of the technical process:*
APAAN to BMK conversion, using of hydrochloric acid, does not require any complex or expensive production equipment. Since hydrochloric acid has a corrosive effect on iron and stainless steel, plastic barrels are used for the conversion reaction. These may vary in size from 80 to 220 L.

The mixing of the reaction mixture of APAAN and hydrochloric acid is not done with electric mixing equipment, as is the case for APAAN conversion with sulphuric acid, but is usually done by hand, using a wooden or plastic stick or spatula.

In most conversion labs that used hydrochloric acid, the set-up resembled the schematic representation below.



​
The two outer barrels are used for the conversion of APAAN to BMK. Tubes protruding from the lids of these barrels lead into the central barrel, which contains a fluid – either a water and caustic soda solution or an alkaline soap – that neutralizes the fumes.

The central barrel may also contain an internal spraying mechanism: A submersible pump in the liquid and a ring of tubing with nozzles immediately under the lid create a mist of the liquid in the barrel. This is done to optimize neutralization and precipitation of the fumes.​

​
The fumes and smell released in filling, mixing and emptying the barrels is extracted by an extractor fan equipped on the front with an active carbon filter.​

​As the reaction between the APAAN and the hydrochloric acid generates now or insufficient heat to complete the conversion to BMK, an external heating source is required. Heating mantles are frequently used for this purpose. In the industrial sector, these mantles are used to heat fluids with a melting point around room temperature for easier transport or processing.


​
The heating mantle can be attached to the plastic barrel, simply using three adjustable straps, after which the desired temperature is set with the aid of a thermostat.





​
*Separation – stage 2.*
After APAAN is converted to BMK, the BMK can be separated off using a separatory funnel or a metal ladle. At that time, the BMK is still acidic and can be neutralized using a caustic soda (NaOH) solution, with a ratio of 25 kg caustic soda in water 50 L.

This reaction will generate heat. In some conversion labs, barrels used for this stage are cooled in metal cooling basins filled with a layer of cooling-water. In the labs in question, the reaction mixture was pumped into plastic barrels in the cooling basins after the first stage: the conversion stage.

After the BMK is neutralized, it can be separated with help of a separatory funnel or a metal ladle.​





​*Purification – stage 3.*
After conversion and neutralization, the BMK is dark brown in, and can subsequently be purified or cleaned using steam distillation or another type of distillation. This distillation removes water and synthesis contaminations (by-products) with boiling points that vary significantly from that of BMK. After distillation, the remaining BMK is pale yellow.​
*Comment:*
The neutralization and purification stages are not essential. The acidic, dark brown coloured BMK can be used as it is for the production of amphetamine and methamphetamine. In some conversion labs, only the conversion process was found, other labs also showed evidence of the neutralization stage.​


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## KokosDreams

What's the recommended route to go from BMK -> Amphetamine Freebase when the BMK was produced with APAAN + Hydrochloric Acid?

Also, what's the final yield of pure Amphetamine Freebase?


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## G.Patton

KokosDreams said:


> What's the recommended route to go from BMK -> Amphetamine Freebase when the BMK was produced with APAAN + Hydrochloric Acid?



KokosDreamsLook around Amphetamines (phenylethylamines). I've already posted this manual.


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## pantona123

First of all thank you for sharing this information, but the apaan I know is a white powder an in the calculation in the top it is measured in litres can I just take 1kg as 1 litre? 
Can I use less solution of caustic soda? 
Thanks in advance and best regards


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## T0R

We're talking about "mole" ratios

The number of moles is obtained by dividing the mass by the molar mass

do you have apaan ?


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## workworkwork

Please manual how to make APAAN!
Is it easily made from Benzyl Chloride and another chemical used in swimming pools that has cyanide in the name? 
Or can I buy APAAN?


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## KokosDreams

workworkwork said:


> Please manual how to make APAAN!
> Is it easily made from Benzyl Chloride and another chemical used in swimming pools that has cyanide in the name?



workworkwork
I would be interested in an APAAN synthesis manual too


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## T0R

workworkwork said:


> Please manual how to make APAAN!
> Is it easily made from Benzyl Chloride and another chemical used in swimming pools that has cyanide in the name?
> Or can I buy APAAN?



workworkworkno you can not
also not for sale becouse it is banned worldwide


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## ASheSChem

workworkwork said:


> Please manual how to make APAAN!



workworkwork


KokosDreams said:


> I would be interested in an APAAN synthesis manual too


don't like this one ? http://bbzzzsvqcrqtki6umym6itiixfhn...oacetonitrile-with-sodium-amide-1kg-scale.60/


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## T0R

ASheSChem said:


> don't like this one ? http://bbzzzsvqcrqtki6umym6itiixfhn...oacetonitrile-with-sodium-amide-1kg-scale.60/



ASheSChem
not realy


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## KokosDreams

ASheSChem said:


> don't like this one ? http://bbzzzsvqcrqtki6umym6itiixfhn...oacetonitrile-with-sodium-amide-1kg-scale.60/



ASheSChemSeems like I haven't seen it or forgot about its existence!

Thanks for the reminder


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## Germinmeth

Very clear and informative. I seem to have understood everything and in the near future I will try to implement this synthesis. Respect to the author! Write more!


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