FIELD: chemistry.
SUBSTANCE: invention relates to a method of producing thymoquinone from black caraway seeds. Method for producing thymoquinone from black caraway seeds, involving triple extraction of fatty oil of black caraway with 70% ethyl alcohol, is characterized by that extraction involves mixing 750 ml of black caraway fatty oil with 150 ml of 70% ethyl alcohol, shaking the obtained mixture for 1-2 minutes, then settling for 20 hours, separating the mixture remaining in the lower layer from the upper layer, then combining and settling the upper layers after the third extraction act for 24 hours, decantation in a two-necked round-bottom flask equipped with a Wurtz nozzle with a thermometer, a straight condenser with an allonge, heating the obtained solution in a glycerine bath to 92 °C and distillation of ethyl alcohol into 250 ml beaker at rate of 1 drop per second at a steam temperature of 74–75 °C, then adding to the two-neck round-bottom flask an equal volume of 96% ethyl alcohol after distillation of each 100 ml, then after three stages of distillation the obtained reaction mass is evaporated in a double-necked round-bottom flask for 250 ml in a vacuum of a rotary evaporator at temperature Tbath=50 °C and pressure P=150 mbar, then heating the reaction mass in a two-necked round-bottom flask equipped with a magnetic anchor, a Wurtz nozzle, a thermometer and a straight condenser with 150 ml of distilled water in a glycerine bath at a temperature of Tbath=115 °C, and mixing at steam temperature Tsteam=97–100 °C, distilling 60 ml of water, then extraction with tert-butyl methyl ether in three steps of 15 ml, drying with sodium sulphate (Na2SO4) and evaporation with an organic solvent in a vacuum of a rotary evaporator at a temperature of Tbath=45 °C and pressure P=180 mbar.
EFFECT: said invention is characterized by output of high concentration of thymoquinone in pure form from black caraway essential oil.
1 cl, 1 tbl
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Authors
Dates
2024-06-25—Published
2023-12-22—Filed