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Triacetoxyperiodinane → 4-Fluoro-3-nitrobenzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triacetoxyperiodinane | HCID 159087 | — |
| 反応物 | 4-Fluoro-3-nitrobenzyl alcohol | HCID 4167587 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Fluoro-3-nitrobenzaldehyde | HCID 598129 | 76.6% |
反応手順
To a stirred solution of (4-fluoro-3-nitro-phenyl)-methanol (750 g, 4.4 mmol) in DCM (40 mL) at 0° C. was added Dess-Martin Reagent (3.0 g, 7 mmol). The solution was stirred at room temperature for 4 hours. TLC showed disappearance of starting material. The reaction was quenched with 10% NaHCO3 and 10% Na2S2O3 aqueous solution and DCM layer separated and washed with water (100 mL) and brine (50 mL). The reaction was concentrated, and the residue was purified by flash chromatography on silica to obtain the title compound (570 mg, yield: 75%). 1H-NMR (400 MHz, DMSO-d6) δ 10.09 (d, 1H), 8.36 (t, 1H), 8.06 (dd, 1H), 7.97 (m, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09434697B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-035f7c5189544f81a4b89988e3a1348d |
| 出典メモ | uspto-grants-2016_09 |