Starting reagents and materialsโ
- 6 g Synthetic ephedrine hydrochloride racemateโ
- 1.8 g Red phosphorous (P)โ
- 12 g Iodine (I2)โ
- 100-150 ml H2Oโ
- 3 g Sodium thiosulfate (Na2S2O3)โ
- 24 ml 25% NaOHโ
- 250-300 ml DCMโ
- 100 ml Petroleum etherโ
- HCl gasโ
- 100 g NH4Clโ
- 25 ml H2SO4 83%โ
- Flasks 250 and 500 ml
- Beakers
- Anhydrous sodium sulfate
- Funnels
- Separating funnel
- Magnetic stirrer with heating
- Flask heater
- Reflux
- Paper filters
- Pipettes
- Porcelain filter for vacuum filtration
- Chen's reagents
- Simon's reagents
- pH indicator paper
โ
The process way presented on Scheme 1.
Starting reagents for meth synthesis: synthetic ephedrine hydrochloride racemate, red P, I2 and H2O. Fig. 1
Ephedrine hydrochloride ground into a powder in a mortar. Fig 2โ
The powder of ephedrine hydrochloride is poured into the flask. Fig 3โ
To the powder of ephedrine hydrochloride, red P are added. Fig 4โ
Ephedrine hydrochloride thoroughly mixed with red P until homogeneous mass. Fig 5โ
Iodine (I2) is grounded into a powder. Fig 6โ
The powder of I2 is added in portions to the mixture in the flask while continuously mixing. Fig 7โ
All components are mixed until a homogeneous mass is obtained. Fig 8โ
Then, water (6 ml) is rapidly added. Fig 9โ
Reflux condenser is connected to the flask, and the mixture is heated at a temperature of 60-80ยฐC for 24 hours. Fig 10โ
To the resulting reaction mixture, 15-20 ml of water is added. Fig 11โ
The reaction mixture is filtered through a paper filter. The filter is additionally washed with water. Fig 12โ
Solution of NaOH added to the filtered solution of RM. Fig 13โ
Then a solution of sodium thiosulfate is added. Fig 14โ
Next, 100 ml of DCM is added. Fig 15โ
The DCM extract is separated. Further, the solution undergoes 2-3 extractions with fresh portions of DCM, each ranging from 20 to 50 ml. Fig 16โ
The DCM is dried over anhydrous sodium sulfate. Fig 17โ
The dried DCM is distilled at a temperature of 90-110ยฐC until the all DCM distilled off. Fig 18โ
To the obtained oil, 30 ml of petroleum ether is added. Fig 19โ
The solution is filtered through a paper filter, and the flask is rinsed with an additional 20-30 ml of petroleum ether. Fig 20โ
Impurities in the form of resin remain on the walls of the flask. Fig 21โ
The filtered solution is saturated with gaseous HCl until it reaches an acidic pH and white precipitate forms. Fig 22โ
The Simon's test for the white precipitate is positive to meth. Fig 23โ
The Chen's reaction for ephedrine is negative in the obtained material. In the right is the test with pure ephedrine - control test. Fig 24โ
To the precipitate, 30 ml of petroleum ether is added and it is filtered through a porous filter. If necessary, it is additionally washed with a portion of petroleum ether and then dried. Fig 25โ
The dry powder of methamphetamine hydrochloride. Fig 26โ
The reaction yield is 4.16 g or 75 %โ
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