関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzenesulfonyl hydrazide | HCID 65723 | — |
| 反応物 | Methyl 4-(4-oxo-chroman-3-ylidenemethyl)-benzoate | HCID 4240115 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 4-(4-oxo-chroman-3-ylmethyl)-benzoate | HCID 22478914 | 42.2% |
反応手順
A suspension of 260 (400 mg, 1.36 mmol) and benzenesulfonyl hydrazine (702 mg, 4.08 mmol) in DMF (7 ml) was stirred at 100° C. during 48 h. The solvent was evaporated and the residue was diluted in AcOEt, washed with NH4Cl sat., brine, dried over anhydrous MgSO4, filtered and concentrated. The crude residue was then purified by flash chromatography on silica gel (5% AcOEt/HEx)to afford the title compound 264 (170 mg, 42%) as a white solid. LRMS: 296.1 (Calc.); 297.0 (found).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07595343B2 |
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| 出典データセット | uspto-grants-2009_09 |
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| ORD ID | ord-1955c810a3794231b42d031e52a40e07 |
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| 出典メモ | uspto-grants-2009_09 |
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