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Tetrahydrofuran → 4-(1-cyclopentyl-7-fluoro-1H-indazol-3-yl)phenyl ethyl hydrogen phosphate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Ethyl dichlorophosphate | HCID 15158 | — |
| 反応物 | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| 反応物 | 4-(1-cyclopentyl-7-fluoro-1H-indazol-3-yl)phenol | HCID 135524867 | — |
| 生成物 | 4-(1-cyclopentyl-7-fluoro-1H-indazol-3-yl)phenyl ethyl hydrogen phosphate | HCID 68883304 | — |
反応手順
A solution of 4-(1-cyclopentyl-7-fluoro-1H-indazol-3-yl)phenol (0.30 g, 1.0 mmol), ethyl dichlorophosphate (0.13 mL, 1.1 mmol), and lithiumhexamethyldisilazide (0.183 g, 1.1 mmol) in 10 mL of THF was stirred for 1 hour at ambient temperature. The reaction mixture was quenched with H2O and concentrated in vacuo. The residues were purified by reversed phase HPLC (Column: HS Hyperprep C18 8 u ID 22 mm; solvent gradient 40% to 100% acetonitrile (0.1% TFA) in H2O; flowrate 10 mL/min) to give 0.065 g of the title compound as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07241791B2 |
| 出典データセット | uspto-grants-2007_07 |
| ORD ID | ord-34d47accdb9343e99da7873dfaab5f30 |
| 出典メモ | uspto-grants-2007_07 |