関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Butyl Acetate | HCID 31272 | — |
| 反応物 | Erythromycin Thiocyanate | HCID 83938 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Erythromycin | HCID 12560 | 15% |
反応手順
A mixture of erythromycin thiocyanate and other impurities (100 g) was added into dichloromethane (300 mL). Butyl acetate (or ethyl acetate) (50 mL) was added, 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 2 hours and then cooled to −5° C. in 16 hours. The crystals formed were filtered. Dichloromethane (20 mL) 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 94.8% with a dichloromethane content of 385 ppm, a water content of 1.1% and a microbiological titre of 943 μ/mg.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08436154B2 |
|---|
| 出典データセット | uspto-grants-2013_05 |
|---|
| ORD ID | ord-1355407117d84a7f877b3bf011280a66 |
|---|
| 出典メモ | uspto-grants-2013_05 |
|---|