Reagents:
Equipment:
Synthesis:
1. Heat the ultrasound bath to 38*C. If your ultrasound bath is without a heating function, you can do this on a hot plate separately.
2. Pour 150mL dichloromethane into a beaker and put in the bath for heating within 5 min.
3. Add 50g of CBD isolate and 1.5g of pTSA and mix until dissolved (or almost complete dissolution).
4. Put the solution in the US-bath and turn on the treatment with ultrasound of 40kHz for 5 minutes. You can see how the boil begins and when the boiling intensity becomes less, then the reaction is finished.
5. Remove the beaker from the US-bath and add 500mL of a concentrated sodium bicarbonate solution. Mix, separate the lower layer through the separatory funnel and repeat the procedure a second time. You can use shaking in a separatory funnel, but do not forget to release gases from the funnel.
6. Add the saturated solution of sodium chloride, mix and separate through the separatory funnel. Repeat the procedure a second time. Do not forget about the evaporation of dichlormethane if you shake in the funnel.
7. Add sodium sulfate, mix the mixture in a beaker and leave for 15 min.
8. Separate the solution from sodium sulfate sediment and pour the solution into the evaporation flask. Recommend decanting the solution, because filtering can be difficult due to the density of the solution.
9. We turn on the vacuum pump and distill at room temperature or heating the rotovap-bath until dichloromethane is completely evaporated. With a high vacuum, do not use the temperature of more than 40-60*C.
10. Remove the resulting oil on a glass dish.
Yield: ~30g. But if you pay more attention to separation (extraction) may be more yield.
The purity is close to the maximum, the ratio of isomers is approximately 40:60 for d9:d8 respectively.
Write any of your questions, we will be happy to answer.
We will continue ultrasonic syntheses in other products and scale.
Expect a video of this synthesis.
- Cannabidiol isolate 50g;
- p-Toluenesulfonic acid (pTSA) 1.5g;
- Dichloromethane 150mL;
- Sodium bicarbonate ~50g;
- Sodium chloride ~100g;
- Sodium sulfate ~10g;
- Dist. H2O 1L;
Equipment:
- Ultrasonic bath (40 kHz with heating);
- Beakers;
- Separatory funnel 2L;
- Rotovap (with vacuum pump and cooling);
- Dishes;
Synthesis:
1. Heat the ultrasound bath to 38*C. If your ultrasound bath is without a heating function, you can do this on a hot plate separately.
2. Pour 150mL dichloromethane into a beaker and put in the bath for heating within 5 min.
3. Add 50g of CBD isolate and 1.5g of pTSA and mix until dissolved (or almost complete dissolution).
4. Put the solution in the US-bath and turn on the treatment with ultrasound of 40kHz for 5 minutes. You can see how the boil begins and when the boiling intensity becomes less, then the reaction is finished.
5. Remove the beaker from the US-bath and add 500mL of a concentrated sodium bicarbonate solution. Mix, separate the lower layer through the separatory funnel and repeat the procedure a second time. You can use shaking in a separatory funnel, but do not forget to release gases from the funnel.
6. Add the saturated solution of sodium chloride, mix and separate through the separatory funnel. Repeat the procedure a second time. Do not forget about the evaporation of dichlormethane if you shake in the funnel.
7. Add sodium sulfate, mix the mixture in a beaker and leave for 15 min.
8. Separate the solution from sodium sulfate sediment and pour the solution into the evaporation flask. Recommend decanting the solution, because filtering can be difficult due to the density of the solution.
9. We turn on the vacuum pump and distill at room temperature or heating the rotovap-bath until dichloromethane is completely evaporated. With a high vacuum, do not use the temperature of more than 40-60*C.
10. Remove the resulting oil on a glass dish.
Yield: ~30g. But if you pay more attention to separation (extraction) may be more yield.
The purity is close to the maximum, the ratio of isomers is approximately 40:60 for d9:d8 respectively.
Write any of your questions, we will be happy to answer.
We will continue ultrasonic syntheses in other products and scale.
Expect a video of this synthesis.
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