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(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 → methyl 1H-benzimidazole-5-carboxylate hydrochloride
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | (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 | — |
| 反应物 | 氯化亚砜 | HCID 24386 | — |
| 反应物 | 1H-苯并咪唑-5-羧酸 | HCID 459456 | — |
| 产物 | methyl 1H-benzimidazole-5-carboxylate hydrochloride | HCID 22710297 | 97% |
反应步骤
Under ice cooling, thionyl chloride (2.30 ml) was added dropwise to methanol (50 ml). Then, 5-benzimidazolecarboxylic acid (5.00 g) was added, followed by heating under reflux for 5 hours. The reaction mixture was distilled under reduced pressure. The residue was pulverized in diethyl ether, followed by collection through filtration, whereby colorless crystals (6.36 g, 97%) was obtained.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US06747023B1 |
| 来源数据集 | uspto-grants-2004_06 |
| ORD ID | ord-f89a7e124718480098b5995cbd3b23e9 |
| 来源说明 | uspto-grants-2004_06 |