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4-Formyl-17beta-estradiol → 4-Formylestrone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Formyl-17beta-estradiol | HCID 11722342 | — |
| 反応物 | Jones' reagent | HCID 131709961 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 4-Formylestrone | HCID 14334327 | 93% |
反応手順
To a solution of 3,17β-dihydroxyestra-1,3,5(10)-triene-4-carboxaldehyde (2b, 0.300 g, 1.0 mmol) in acetone (10 mL) was added Jones reagent (0.50 mL) at 0° C. The reaction mixture was stirred for 10 min, quenched with 2-propanol, and extracted with EtOAc. The combined organic layers were washed with H2O, then with saturated aqueous NaCl, and dried (Na2SO4). The desiccant was filtered and the solvent was evaporated at reduced pressure. The residue was purified by column chromatography (silica gel) using n-hexane:THF (4:1→2:1, v/v) to afford 0.276 g of 12 (93% yield), m.p. 234°-237° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05861388 |
| 出典データセット | uspto-grants-1999_01 |
| ORD ID | ord-ce95a65df00c40ad932a9a570aa9ef88 |
| 出典メモ | uspto-grants-1999_01 |