Method for preparing beta-artemether artemether from artemether mother liquor
A technology of artemether and refining method, which is applied in the field of preparation of β-artemether, can solve the problems of difficult large-scale implementation of chromatography technology, no obvious use value of α-artemether, low conversion and refining efficiency, etc. Achieve the effect of convenient operation, good product purity and waste reduction
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Embodiment 1
[0025] Concentrate the crystallization mother liquor of artemether prepared from dihydroartemisinin until viscous, separate by column chromatography to obtain α-artemether solution, evaporate to remove the organic solvent, and then dry at 50°C until constant weight to obtain crystals.
[0026] In a clean 15L reactor, add 2000ml of toluene, 6000ml of dichloromethane and 1600ml of methanol, plus 800g of the above-mentioned crystals (the content of α-artemether is 90% and the content of β-artemether is 10% as detected by HPLC), Stir to dissolve at 30°C. Add 24g of p-toluenesulfonic acid and stir for 3 hours. Let stand for 0.5 hour, filter, and wash the filtrate with 2800ml of water. After adding 20g of anhydrous magnesium sulfate to dry, shrink the filtrate to dryness to obtain a total of 530g of extract. The concentrate was added to methanol, dissolved at 50°C to form a saturated solution, transferred to an ice-water bath to stir and crystallize for 1 hour, filtered with sucti...
Embodiment 2
[0029] Concentrate the crystallization mother liquor of artemether prepared from dihydroartemisinin until viscous, separate by column chromatography to obtain α-artemether solution, evaporate to remove the organic solvent, and then dry at 50°C until constant weight to obtain crystals.
[0030] In a clean 15L reactor, add 1920ml of toluene, 7680ml of dichloromethane and 1800ml of methanol, plus 800g of the above-mentioned crystals (the content of α-artemether is 90% and the content of β-artemether is 10% as detected by HPLC), Stir to dissolve at 30°C. Add 20g p-toluenesulfonic acid to react for 3 hours. Let stand for 0.5 hour, filter, and wash the filtrate with 3000ml of water. After adding 20g of anhydrous magnesium sulfate and drying, the filtrate was concentrated to an extract. The concentrate was added to methanol, dissolved at 50°C to form a saturated solution, transferred to an ice-water bath, stirred and crystallized for 1 hour, filtered with suction, and dried at 50°C...
Embodiment 3
[0034] Concentrate the artemether mother liquor produced by dihydroartemisinin into artemether and filter and wash it in vacuum at 40°C under reduced pressure, evaporate most of the methanol, and then dry it at 50°C to constant weight to obtain Crystal, take 800g of crystal for later use.
[0035] In a clean 15L reactor, add 2000ml of toluene, 8000ml of dichloromethane and 2500ml of methanol, and then add 800g of crystals (the content of α-artemether is 87% and the content of β-artemether is 13% as detected by HPLC). Stir to dissolve at 32°C. Add 30g p-toluenesulfonic acid to react for 3 hours. Let stand for 0.5 hour, filter, and wash the filtrate with 3000ml of water. After adding 20g of anhydrous magnesium sulfate and drying, the filtrate was concentrated to an extract. The concentrate was added to methanol, dissolved at 50°C to become a saturated solution, transferred to an ice-water bath to stir and crystallize for 1 hour, filtered with suction, and dried at 50°C to con...
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