Starting reagents and materials
- 6 g Synthetic ephedrine hydrochloride racemate
- 1.8 g Red phosphorous (P)
- 12 g Iodine (I2)
- 100-150 ml H2O
- 3 g Sodium thiosulfate (Na2S2O3)
- 24 ml 25% NaOH
- 250-300 ml DCM
- 100 ml Petroleum ether
- HCl gas
- 100 g NH4Cl
- 25 ml H2SO4 83%
- 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
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 2
The powder of ephedrine hydrochloride is poured into the flask. Fig 3
To the powder of ephedrine hydrochloride, red P are added. Fig 4
Ephedrine hydrochloride thoroughly mixed with red P until homogeneous mass. Fig 5
Iodine (I2) is grounded into a powder. Fig 6
The powder of I2 is added in portions to the mixture in the flask while continuously mixing. Fig 7
All components are mixed until a homogeneous mass is obtained. Fig 8
Then, water (6 ml) is rapidly added. Fig 9
Reflux condenser is connected to the flask, and the mixture is heated at a temperature of 60-80°C for 24 hours. Fig 10
To the resulting reaction mixture, 15-20 ml of water is added. Fig 11
The reaction mixture is filtered through a paper filter. The filter is additionally washed with water. Fig 12
Solution of NaOH added to the filtered solution of RM. Fig 13
Then a solution of sodium thiosulfate is added. Fig 14
Next, 100 ml of DCM is added. Fig 15
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 16
The DCM is dried over anhydrous sodium sulfate. Fig 17
The dried DCM is distilled at a temperature of 90-110°C until the all DCM distilled off. Fig 18
To the obtained oil, 30 ml of petroleum ether is added. Fig 19
The solution is filtered through a paper filter, and the flask is rinsed with an additional 20-30 ml of petroleum ether. Fig 20
Impurities in the form of resin remain on the walls of the flask. Fig 21
The filtered solution is saturated with gaseous HCl until it reaches an acidic pH and white precipitate forms. Fig 22
The Simon's test for the white precipitate is positive to meth. Fig 23
The Chen's reaction for ephedrine is negative in the obtained material. In the right is the test with pure ephedrine - control test. Fig 24
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 25
The dry powder of methamphetamine hydrochloride. Fig 26
The reaction yield is 4.16 g or 75 %
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