Synthesis of 4-MAR (4 -methyl-aminorex)

strannik

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Two components are needed for synthesis: phenylpropanolamine hydrochloride (PPA.HCl) and potassium cyanate (KOCN). The first one was extracted from an absolutely legal remedy for cats and dogs - Propalin (the price is 380 rubles per bottle, in which 5 g of PPA.HCl,

The chop of phenylpropanolamine", the second one is made from alkali (KOH) and urea, the price of both is within one hundred rubles per kilogram, it is sold freely. However, potassium cyanate can be bought at the rate of 500 rubles per 100 grams, it is legally sold. Potassium cyanate, unlike potassium cyanide (KCN), is not fatal, but this does not mean at all that it should be dragged into the mouth with spoons.

1. PHENYLPROPANOLAMINE HYDROCHLORIDE (PPA.HCl).

PPA.HCl was obtained by acid-base extraction (KSHE) from Propalin, which, in turn, was purchased at a veterinary pharmacy (see Yandex, who needs it). The yield is 2.4 g out of 10 g in two vials of syrup (there were shoals due to the density of the syrup, so the yield is low). Hydrochloride was planted from IPS, crystallizes perfectly, the color is white. It is washed once with acetone.

P.S. The authenticity of phenylpropanolamine was verified by biotesting a product obtained by a conventional screw reaction (PPA.HCl + iodine + red phosphorus = amphetamine + dirt).

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2. POTASSIUM CYANATE (KOCN).

10 g (166.5 mol) of urea (the second name is carbamide, MW = 60.05) is dissolved in 70 ml of water, 17.8 g (317.5 mol) KOH (MW = 56.11) is dissolved in dry form and boiled under a reverse refrigerator for 30 minutes (ammonia is released). Then the solution is poured into a frying pan and the liquid is evaporated. Ammonia and carbon dioxide continue to be abundantly released. Then the temperature is raised to 180...240 degrees. The mixture hardens again, it is crushed and the reaction continues for another 1.5 hours at this temperature. After cooling, the product is crushed and washed with acetone. The slightly beige crystals obtained are dried and stored in a closed container, they can be recrystallized from boiling water. The yield is 10.7 g (79.2%). Potassium cyanate KOCN (MW=81.11) has a density of 2.03, a melting point of 315 degrees, solubility in water - 38.6, insoluble in ethanol, acetone.
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3. 4-MAR.

2.4g (12.7 mmol) PPA.HCl is mixed with 1.2 g (14.8 mmol) KOCN and placed in a flask. Add 50 ml of water and, after dissolution, boil it under a reverse refrigerator for 2 hours. The mixture is allowed to cool slightly and 20 ml of concentrated hydrochloric acid is added in small portions to 70 ml of water. There is a slight gas release from the decomposition of cyanate residues. When the addition is completed, the mixture continues to boil under the reflux refrigerator for 6 hours. About three hours after adding the acid, the mixture acquires a slightly pink tint - this is a sign of the beginning of product formation, it is worth paying attention to.

After the specified time, the mixture is allowed to cool down and carefully alkalized (the reaction is slightly exothermic). At the same time, white crystals of the 4-MAR base fall out. The crystals are filtered, washed with small amounts of cold alkaline water and dried. The yield is 1.7 g (70%).

It was not possible to obtain hydrochloride (it did not crystallize from IPS), the substance was returned to the base form.


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5. BIOTESTS.

The bioassays were convincing, the substance is clearly felt in a dosage of 15 mg, the average dose is 40 mg, an overdose begins from 60 mg. Tested on the stomach, by smoking and intravenously. Of the distinctive features, the following is noted:

the closest analogue in terms of effects is methamphetamine
 
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HIT MONKEY

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2.4 g PPA.HCl (12.7 mmol) is mixed with 1.2 g KOCN (14.8 mmol) in a vial. Add 50 mL of water and dissolve. Place in the refrigerator in reverse order for 2 hours.
(Question)🙋=What is reverse boiling in a refrigerator?
Or do you mean an exothermic chemical reaction?
 

strannik

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this refers to boiling with a deflegmator
 

frolov_semen

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Hey! How you obtained PPA.HCl 2.4 g via acid-base extraction (KSHE) from 10 g Propalin? How do you think you can increase your yields?
 
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