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Potassium Carbonate → HCID 82810771、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Fluoro-3-methoxybenzaldehyde | HCID 3774463 | — |
| 反応物 | Dimethyl-1-diazo-2-oxopropylphosphonate | HCID 86586111 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 82810771 | HCID 82810771 | 92.2% |
反応手順
Potassium carbonate (3.6 g, 26.0 mmol) and dimethyl-1-diazo-2-oxopropylphosphonate (2.4 mL, 15.6 mmol) were added sequentially to a solution of 2-fluoro-3-methoxybenzaldehyde (2.0 g, 13.0 mmol) in methanol (100 mL), and the reaction was allowed to stir at room temperature for 16 h. After concentrating the reaction mixture under reduced pressure, the crude material was purified by flash chromatography (40 g silica gel column, 0-40% gradient ethyl acetate in hexanes) to provide a clear colorless oil (1.8 g, 92%). MS (GCMS) m/z 150. 1H NMR (400 MHz, CHLOROFORM-d) δ3.31 (d, J=0.78 Hz, 1H) 3.90 (s, 3H) 6.93-7.11 (m, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08748466B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-0ee9c85b54f14a6d9bf2444ee02b6e73 |
| 出典メモ | uspto-grants-2014_06 |