Reagents:
- Lysergic acid (cas 82-58-6)2.80 g;
- Methylene chloride (DCM; CH2Cl2) 190 ml;
- N,N-Diethylmethylamine (cas cas 616-39-7) 1.81 g;
- PyBOP (cas 128625-52-5) 5.70 g;
- Diethylamine (cas 109-89-7) 0.84 g;
- Ammonium hydroxide (NH4OH) 100 ml 7.5 M;
- Sodium bicarbonate (cold saturated aq solution) NaHCO3 40 ml;
- Ethyl acetate (EtOAc) 60 ml;
- Sodium sulphate (MgSO4) ~50 g;
- Deionized H2O ~200 ml;
Equipment and glassware:
- Round bottom flask 250 mL;
- Retort stand and clamp for securing apparatus;
- Magnetic stirrer;
- Separatory funnel 500 mL (optional);
- Glass rod and spatula;
- Laboratory scale (0.1-100 g is suitable);
- Measuring cylinder 100 mL;
- Funnel;
- Filter paper;
- Rotovap machine (optional);
- Vacuum source;
- Buchner flask and funnel;
- Beakers 100 ml x2 and 250 ml x2;
Lysergic acid 2.80 g is added to a methylene chloride (DCM; CH2Cl2) 100 ml with a constant stirring. N,N-Diethylmethylamine 1.81 g is added to the reaction mixture and the solution is stirred for 5 min. Then PyBOP 5.70 g is added, and the solution is stirred for an additional 5 min. Then, diethylamine 0.84 g is added and the reaction is stirred at room temperature for 60 min.
The reaction mixture is quenched with concentrated ammonium hydroxide (NH4OH) 100 ml 7.5 M. Layers are separated, the aqueous phase is extracted with 3x30 ml DCM. Organic layers are combined and evaporated in a rotovap machine at 35 °C under high vacuum.
The residue is dissolved in sodium bicarbonate (cold saturated aq solution) NaHCO3 40 ml and extracted with 3x20 ml EtOAc. Organic layers are combined and washed with deionized H2O, brine, and dried over MgSO4. Solution is filtered and evaporated in a rotovap machine at 40 °C under vacuum to a constant weight. A yield is 3.13 g before chromatography purification (optional), 93% purity.
The reaction mixture is quenched with concentrated ammonium hydroxide (NH4OH) 100 ml 7.5 M. Layers are separated, the aqueous phase is extracted with 3x30 ml DCM. Organic layers are combined and evaporated in a rotovap machine at 35 °C under high vacuum.
The residue is dissolved in sodium bicarbonate (cold saturated aq solution) NaHCO3 40 ml and extracted with 3x20 ml EtOAc. Organic layers are combined and washed with deionized H2O, brine, and dried over MgSO4. Solution is filtered and evaporated in a rotovap machine at 40 °C under vacuum to a constant weight. A yield is 3.13 g before chromatography purification (optional), 93% purity.
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