関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Erythromycin Thiocyanate | HCID 83938 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Erythromycin | HCID 12560 | 15% |
反応手順
A mixture of erythromycin thiocyanate and other impurities (100 g) was added into a solvent mixture (300 mL) comprising dichloromethane and acetone (the volume content of dichloromethane is 60%), stirred under heat to 34° C. and adjusted to pH 12 until the solution became clear. The upper aqueous phase was separated and removed to obtain a dichloromethane solution with about 15% of erythromycin A. The dichloromethane solution was cooled to 23° C., kept for one hour and then cooled to 3° C. in 16 hours. The crystals formed were filtered. Dichloromethane (20 mL) (the content of dichloromethane is 95% and ethanol is 5%) was used to wash the crystals and the crystals were filtered for further 5 minutes. The amount of erythromycin A in the dried erythromycin is 94.6% with a dichloromethane content of 352 ppm, a water content of 2.2% and a microbiological titre of 941 μ/mg.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08436154B2 |
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| 出典データセット | uspto-grants-2013_05 |
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| ORD ID | ord-c9bdf1dbb5f7473cbb54edd3d6cee7b4 |
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| 出典メモ | uspto-grants-2013_05 |
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