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Potassium Nitrate → Previtamin D3
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Nitrate | HCID 24434 | — |
| 反応物 | (24R)-5,7-Ergostadiene-1alpha,3beta,25-triol | HCID 23239490 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Previtamin D3 | HCID 5281058 | 28.3% |
反応手順
(24R)-5,7-Ergostadiene-1α,3β,25-triol (IIb) (100 mg, 0.23 mmol) prepared in Example 13 was dissolved in ether (1000 ml) and the solution was irradiated for 3 minutes with high pressure mercury lamp using 1.5% aqueous potassium nitrate solution as a filter under water-cooling in an argon gas stream. From the reaction solution was distilled off ether and the resultant residue was purified by preparative high performance liquid chromatography (HPLC) [column: LiChrosorb® Si60 (7 μm), φ25×250 mm, Merck Co., Ltd.; column effluent: 6% methanol-methylene chloride; flow rate: 6.0 ml/ml, detected at 265 nm] to give 25.0 mg of previtamin D (XIIb).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05157135 |
| 出典データセット | uspto-grants-1992_10 |
| ORD ID | ord-33c56a26ac424946bb04bdff58915a7d |
| 出典メモ | uspto-grants-1992_10 |