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Ammonia → N-Demethylerythromycin A
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Erythromycin | HCID 12560 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Methanol--water (1/1) | HCID 22242641 | — |
| 生成物 | N-Demethylerythromycin A | HCID 10010092 | 40.8% |
反応手順
5 g of erythromycin A and 4.7 g of sodium acetate (×3 H2O) were dissolved in 200 ml of an 8:2 methanol/water mixture. 1.75 g of iodine were added to the solution, and the reaction mixture was then irradiated with a quartz lamp at room temperature for 20 minutes. Subsequently, half the solvent was evaporated, and the remaining reaction mixture was poured into a mixture of 140 ml of water and 10 ml of ammonia. The reaction mixture was extracted three times with 20 ml portions of methyl t-butyl ether. The ether extract was separated and some of the ether was evaporated. The reaction product was then left to crystallize out and was recrystallized from acetone. 2 g of N-demethylerythromycin A were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05418224 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-a5e8b30eff0043a4993d87753dbbf392 |
| 出典メモ | uspto-grants-1995_05 |