関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 反応物 | 4-Fluoro-3-(hydroxymethyl)benzeneboronic acid | HCID 21865588 | — |
| 反応物 | 3-bromo-5-nitro-1-trityl-1H-indazole | HCID 58946443 | — |
| 触媒 | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| 溶媒 | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| 生成物 | 3-(4-fluoro-3-hydroxymethylphenyl)-5-nitro-1-trityl-1H-indazole | HCID 68964219 | — |
反応手順
A suspension of 3-bromo-5-nitro-1-trityl-1H-indazole 1 (6 g, 12.41 mmol), 4-fluoro-3-hydroxymethylphenylboronic acid 10AV (2 g, 12.87 mmol), Pd(dppf)Cl2 (800 mg, 0.98 mmol) and K3PO4 (6 g, 28.30 mmol) in 124 mL of dioxane/H2O (25:6) was heated to 80° C. for overnight. After removal of most of the solvent, the black residue was diluted with EtOAc (250 mL) and H2O (60 mL). The resulting mixture was filtered through a pad of Celite. Additional 150 mL of EtOAc was used to wash the Celite cake. The filtrates were combined. The aqueous layer was separated and the organic layer was washed with brine, dried (MgSO4) and concentrated to give crude 3-(4-fluoro-3-hydroxymethylphenyl)-5-nitro-1-trityl-1H-indazole 11AV (8.2 g) as a greenish yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08546404B2 |
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| 出典データセット | uspto-grants-2013_10 |
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| ORD ID | ord-4be6f1cbf11b45cbb6cf329ee40e6899 |
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| 出典メモ | uspto-grants-2013_10 |
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