Extraction of ephedra alkaloids from plant material involved weighing ground ephedra, adding an aqueous KOH solution, NaCl, and diethyl ether, shaking and centrifuging. The diethyl ether was collected and dried, with reported alkaloid recovery of 96.6-100.1%. Synthesizing methamphetamine began with washing ground ephedra three times with methanol to produce a greenish-brown substance. This was added to hydriodic acid and red phosphorus, heated and refluxed for 5 hours. The reaction solution was filtered, extracted, dried, treated with HCl gas to crystallize the final hydrochloride salt product. Samples were taken throughout and analyzed.
Extraction of ephedra alkaloids from plant material involved weighing ground ephedra, adding an aqueous KOH solution, NaCl, and diethyl ether, shaking and centrifuging. The diethyl ether was collected and dried, with reported alkaloid recovery of 96.6-100.1%. Synthesizing methamphetamine began with washing ground ephedra three times with methanol to produce a greenish-brown substance. This was added to hydriodic acid and red phosphorus, heated and refluxed for 5 hours. The reaction solution was filtered, extracted, dried, treated with HCl gas to crystallize the final hydrochloride salt product. Samples were taken throughout and analyzed.
Extraction of ephedra alkaloids from plant material involved weighing ground ephedra, adding an aqueous KOH solution, NaCl, and diethyl ether, shaking and centrifuging. The diethyl ether was collected and dried, with reported alkaloid recovery of 96.6-100.1%. Synthesizing methamphetamine began with washing ground ephedra three times with methanol to produce a greenish-brown substance. This was added to hydriodic acid and red phosphorus, heated and refluxed for 5 hours. The reaction solution was filtered, extracted, dried, treated with HCl gas to crystallize the final hydrochloride salt product. Samples were taken throughout and analyzed.
Extraction of ephedra alkaloids from plant material involved weighing ground ephedra, adding an aqueous KOH solution, NaCl, and diethyl ether, shaking and centrifuging. The diethyl ether was collected and dried, with reported alkaloid recovery of 96.6-100.1%. Synthesizing methamphetamine began with washing ground ephedra three times with methanol to produce a greenish-brown substance. This was added to hydriodic acid and red phosphorus, heated and refluxed for 5 hours. The reaction solution was filtered, extracted, dried, treated with HCl gas to crystallize the final hydrochloride salt product. Samples were taken throughout and analyzed.
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(From Ma Huang Plant Material)
Extraction of Ephedra Alkaloids From the Crude Drug
An aliquot of 200 mg of the ground ephedra plant material was weighed into a 15 mL centrifuge tube. Two mLs of aqueous 0.65 M KOH solution, 1.2 grams of NaCl, and 2.0 mL of diethyl ether were added to the tube, shaken for two minutes and centrifuged. The diethyl ether was collected and dried over sodium sulfate. Reported alkaloid recovery was 96.6-100.1%4. To 1.0 mL of the diethyl ether was added 1.0 mL of a 0.26 mg/mL solution of n-pentadecane in methylene chloride (CH2Cl2) as an internal standard.
Synthesizing Methamphetamine with Ephedra
Approximately 425 grams of ground ephedra plant material was washed three times with methanol. The methanol washings were collected and allowed to evaporate to produce a greenish-brown tar-like substance. To this material was added 250 mL of a 57% solution of hydriodic acid and 9.5 grams of red phosphorus in a 1000 mL round-bottom flask. The flask was equipped with a working condensor and a heating mantle. The mixture was heated and allowed to reflux for approximately 5 hours. The aqueous reaction solution was filtered, made basic with NaOH (pH>12), then extracted into trichlorotrifluoroethane (Freon-113). The organic solution was dried over anhydrous Na2SO4. Hydrogen chloride gas was then bubbled into the freon, resulting in the crystallization of the final product as the hydrochloride salt8,12. Samples of the reaction mixture were taken at various times throughout the synthesis. These samples were basified, extracted into methylene chloride, and analyzed on the GC-IRD and GC-MSD. Samples were taken at 60, 127, and 310 minutes into the reaction synthesis.
Atom Economical Synthesis of 4'-Methylpropiophenone by Friedel-Crafts Acylation of Toluene With Propionic Anhydride Over Solid Me So Porous Superacid UDCaT-5
