化工社化工社化学信息打印报告 · 仅供科研参考
5-[(2-(3-Phenylpropionyl)-5-pyridyl)methylene]thiazolidine-2,4-dione → 5-[(2-(3-Phenyl-1-hydroxypropyl)-5-pyridyl)methyl]thiazolidine-2,4-dione
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 5-[(2-(3-Phenylpropionyl)-5-pyridyl)methylene]thiazolidine-2,4-dione | HCID 54315938 | — |
| 催化剂 | 钠汞齐 | HCID 9837419 | — |
| 溶剂 | (5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮 | HCID 887 | — |
| 产物 | 5-[(2-(3-Phenyl-1-hydroxypropyl)-5-pyridyl)methyl]thiazolidine-2,4-dione | HCID 14459935 | 36% |
反应步骤
To a solution of the title product of Example 67 (260 mg, 0.77 mmol) in methanol (10 ml) was added 3% sodium amalgam (4 g) and the reaction was stirred for 4 hours. The methanol was decanted, evaporated and the resultant solid diluted with water (10 ml). The aqueous solution was adjusted to pH 2 with 1N HCl and extracted with CH2Cl2 (3×10 ml) which was discarded. After neutralization of the aqueous layer to pH 7 with NaHCO3, it was then re-extracted with CH2Cl2 (3×10 ml). These combined organic layers were dried (MgSO4), filtered and concentrated to afford the desired product (94 mg, 36%) isolated as a foam.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US05223522 |
| 来源数据集 | uspto-grants-1993_06 |
| ORD ID | ord-e5335dbb85c140e1b30e8891097a3e0d |
| 来源说明 | uspto-grants-1993_06 |