A kind of preparation method of ergonovine
A technology of ergometrine and lysergic acid, applied in directions such as organic chemistry, can solve the problems such as the lack of a better treatment method for waste materials, and achieve the effects of offsetting costs, simple method, and no splitting process.
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Embodiment 1
[0045] Embodiment 1: Preparation of lysergic acid
[0046] Accurately weigh 50 g of waste material, add 100 mL of ethanol and stir to dissolve, then add NaOH solid (30 g) and water (500 mL) in sequence. The above reaction mixture was stirred overnight at 80 °C. After cooling to room temperature, concentrate to remove ethanol and add water (500mL) to dilute, the system is acidified with 40% sulfuric acid to pH=3.5-4.0, a large amount of solid precipitates out, and a dark black crude product is obtained by suction filtration. The dark black solid crude product was extracted 3 times with methanol / ammonia water (v / v=95 / 5,500mL / time), the extract was concentrated to dryness, and the obtained gray solid was beaten once with water (500mL) and twice with methanol (300mL) to obtain 12 g of off-white solid. According to HPLC and HNMR analysis, the product was a mixture of lysergic acid and isolysergic acid in a ratio of 1:1.
Embodiment 2
[0047] Embodiment 2: preparation lysergic acid
[0048] Accurately weigh 50 g of waste material, add 100 mL of ethanol and stir to dissolve, then add KOH solid (42 g) and water (500 mL) in sequence. The above reaction mixture was stirred overnight at 80 °C. After cooling to room temperature, concentrate to remove ethanol and add water (500mL) to dilute, the system is acidified with 40% sulfuric acid to pH=3.5-4.0, a large amount of solid precipitates out, and a dark black crude product is obtained by suction filtration. The dark black solid crude product was extracted 3 times with methanol / ammonia water (v / v=95 / 5,500mL / time), the extract was concentrated to dryness, and the obtained gray solid was beaten once with water (500mL) and twice with methanol (300mL) to obtain 8 g off-white solid. According to HPLC and HNMR analysis, the product was a mixture of lysergic acid and isolysergic acid in a ratio of 1:1.
Embodiment 3
[0049] Embodiment 3: preparation lysergic acid
[0050] Accurately weigh 50 grams of waste material, add 100 mL of ethanol and stir to dissolve, then add NaOH solid (96 g) and water (500 mL) in sequence. The above reaction mixture was stirred overnight at 80 °C. After cooling to room temperature, concentrate to remove ethanol and add water (500mL) to dilute, the system is acidified with 40% sulfuric acid to pH=3.5-4.0, a large amount of solid precipitates out, and a dark black crude product is obtained by suction filtration. The crude dark black solid was extracted three times with methanol / ammonia (v / v=95 / 5,500mL / time), the extract was concentrated to dryness, and the obtained gray solid was beaten once with water (500mL) and twice with methanol (300mL) to obtain 12 g off-white solid. According to HPLC and HNMR analysis, the product was a mixture of lysergic acid and isolysergic acid in a ratio of 1:1.
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