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左旋甲状腺素EP杂质H → 3-[(4-fluoro-1H-indol-3-yl)methyl]-2-thioxo-1,2,3,7-tetrahydro-6H-purin-6-one
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 左旋甲状腺素EP杂质H | HCID 6451352 | — |
| 反应物 | tert-butyl 4-fluoro-3-[(6-oxo-2-thioxo-1,2,6,7-tetrahydro-3H-purin-3-yl)methyl]-1H-indole-1-carboxylate | HCID 86631124 | — |
| 溶剂 | 二氯甲烷 | HCID 6344 | — |
| 产物 | 3-[(4-fluoro-1H-indol-3-yl)methyl]-2-thioxo-1,2,3,7-tetrahydro-6H-purin-6-one | HCID 24855501 | 42.3% |
反应步骤
A solution of tert-butyl 4-fluoro-3-[(6-oxo-2-thioxo-1,2,6,7-tetrahydro-3H-purin-3-yl)methyl]-1H-indole-1-carboxylate (0.089 g, 0.21 mmol, obtained from Example 11(c)) in CH2Cl2:TFA 4:1 (1 mL) was stirred for 1 h 40 minutes and then evaporated. The crude product was purified by preparative HPLC, giving the title compound (0.028 g, 42%) as a solid.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US08026244B2 |
| 来源数据集 | uspto-grants-2011_09 |
| ORD ID | ord-5dfd4f60facf438d8f3a6c26c5f9565f |
| 来源说明 | uspto-grants-2011_09 |