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Dexamethasone → Deltasol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dexamethasone | HCID 5743 | — |
| 反応物 | Succinic anhydride | HCID 7922 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | Deltasol | HCID 235849 | — |
反応手順
An amount equivalent to 0.030 g of dexamethasone (1, 0.076 mmol, 1.0 equiv.) was completely dissolved in 1 mL of pyridine (non-anhydrous) and 0.038 g of succinic anhydride (0.382 mmol, 5.0 equiv.) was added to the clear solution. Then 1-2 mg of DMAP (7.6 μmol, 0.1 equiv.) was added to the solution and reaction was allowed to run for 48 h at r.t. under N2-flow. After 48 h, pyridine was evaporated under reduced pressure (in a rotary evaporator). A volume equivalent to 10 mL of H2O was added to the evaporated residue. A white precipitate was observed which was stirred for 10 minutes and then centrifuged. The resulting precipitate was washed again with 10 mL of H2O and the washed residue was lyophilized to yield the target product (2).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09289506B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-2a33efbe14884b429230be4adb88a565 |
| 出典メモ | uspto-grants-2016_03 |