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3,3',5,5'-Tetraiodothyroformic acid → 3-[(4-fluoro-1H-indol-3-yl)methyl]-2-thioxo-1,2,3,7-tetrahydro-6H-purin-6-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3,3',5,5'-Tetraiodothyroformic acid | HCID 6451352 | — |
| 反応物 | 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 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-[(4-fluoro-1H-indol-3-yl)methyl]-2-thioxo-1,2,3,7-tetrahydro-6H-purin-6-one | HCID 24855501 | 42.3% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08026244B2 |
| 出典データセット | uspto-grants-2011_09 |
| ORD ID | ord-5dfd4f60facf438d8f3a6c26c5f9565f |
| 出典メモ | uspto-grants-2011_09 |