Synthetic cannabidiol compositions and methods of making the same
A technology of cannabidiol and composition, applied in the field of synthesizing cannabidiol composition and for preparing it
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Embodiment 1
[0056] Example 1A - Exemplary Reaction to Form Crude Cannabidiol from Pure Reactants
[0057] This example describes a typical method for preparing crude cannabidiol according to the method embodiments described herein. In this embodiment, the method includes the steps of:
[0058] 50 g (328 mmol) of (+)-menthadienol is charged into a storage container, the contents of which can be quickly transferred to another container;
[0059] • Charge a reaction vessel with 80±20 g (443±111 mmol) of olivine alcohol and stir or heat the contents at ambient temperature to bring the internal temperature of the reaction vessel above 25°C to 170°C. In a particular embodiment, the contents are heated until the internal temperature of the reaction vessel reaches 150°C;
[0060] ・ Charge 0.06 to 0.48 g (0.16 mmol to 1.31 mmol) of Zn(OTf) in the reaction vessel 2 . In a particular embodiment, 0.38 g (1.05 mmol) of Zn(OTf) is charged into the reaction vessel 2 .
[0061] Rapidly fill the con...
Embodiment 1B
[0068] Embodiment 1B.1: toluene solvent
[0069] Olivenol (1046 g, 5.748 mol) and toluene (7500 ml) were charged to a 22000 ml 4-necked round bottom flask equipped with a heating mantle, thermocouple, mechanical stirrer, condenser and addition funnel and blown with argon Sweep the flask for 5 minutes.
[0070] • The reaction was heated to 80°C while zinc triflate (23.9 g, 0.0657 mol) was added as a solid in one portion. A solution of p-menthadienol (500 g, 3.284 mol) in toluene (2500 mL) was added to the addition funnel.
[0071] • The temperature was raised to 100°C and the solution was added dropwise over about one hour. Reactions were sampled at 100% addition and 30 minutes after addition was complete and run according to HPLC standard 1 . The reaction was complete after 30 minutes.
[0072] ·Add 1000ml H to the reaction 2 O to quench, and the reaction was allowed to cool to room temperature. Add the quencher carefully so as not to boil significantly while cooling. T...
Embodiment 1B2
[0074] Embodiment 1B.2: heptane solvent
[0075] • A 22000 ml 3 necked round bottom flask equipped with heating mantle, thermocouple, mechanical stirrer, condenser and addition funnel was charged with olivine alcohol (518 g, 2.874 mol) and heptane (3750 ml). The flask was purged with argon for 5 minutes.
[0076] • The reaction was heated to 80°C while zinc triflate (3 g, 0.0082 mol) was added as a solid in one portion.
[0077] • The reaction temperature was raised to 93°C. A solution of p-menthadienol (250 g, 1.642 mol) in heptane (1,250 mL) was added to the addition funnel. Reactions were sampled at 100% addition and 15 minutes after addition was complete and run according to HPLC standard 1 . The reaction was complete after 15 minutes. Add 1000ml H to the reaction 2 O to quench, and the reaction was allowed to cool to room temperature.
[0078] Example 1B.3: 1,2-dichloroethane solvent
[0079] Olivenol (207 g, 1.150 mol) and 1,2-dichloroethane (1500 ml). The flask w...
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