関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methylprednisolone | HCID 6741 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 6alpha-Methylhydrocortisone | HCID 102147 | 94.2% |
反応手順
In a 250 mL round-bottomed flask was suspended (6S,8S,9S,10R,11S,13S,14S,17R)-11,17-dihydroxy-17-(2-hydroxyacetyl)-6,10,13-trimethyl-6,7,8,9,10,11,12,13,14,15,16,17-dodecahydro-3H-cyclopenta[a]phenanthren-3-one (6α-Methylprednisolon, 4.3 g, 11.48 mmol) in EtOAc (80 mL) and the reaction mixture was diluted with ethanol (20.0 mL). Tris(triphenylphosphine)rhodium(I)chloride (Wilkinson's catalyst, 1 g, 1.08 mmol) was added together with a magnetic stirrer bar and the flask was vigorously stirred in a hydrogen atmosphere (1 atm) at room temperature for 1 week. The reaction mixture was filtered through a glass filter funnel and the filtrate was concentrated in vacuo to yield 4.07 g of the desired compound as a light brown solid which was used in the next step without any further purification. APCI-MS m/z: 377 [MH+].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08338587B2 |
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| 出典データセット | uspto-grants-2012_12 |
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| ORD ID | ord-4c6e88d4b42f4559993ff64ccdad5539 |
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| 出典メモ | uspto-grants-2012_12 |
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