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Water → 2-(1,3-Dimethoxy-1,3-dioxopropan-2-yl)-4-nitrobenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Chloro-4-nitrobenzoic acid | HCID 7448 | — |
| 反応物 | Dimethyl malonate | HCID 7943 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 触媒 | copper(I) bromide | HCID 24593 | — |
| 生成物 | 2-(1,3-Dimethoxy-1,3-dioxopropan-2-yl)-4-nitrobenzoic acid | HCID 10590078 | 68% |
反応手順
2-Chloro-4-nitrobenzoic acid (7.5 g, 37.2 mmol) was dissolved in deaerated dimethyl malonate (90 mL). Copper (I) bromide (0.54 g, 3.7 mmol) and sodium methoxide (4.83 g, 89.4 mmol) were added to the solution. The mixture was stirred at room temperature for 15 minutes, and then stirred at 70 to 75° C. overnight. After the reaction solution was allowed to return to room temperature, water was added thereto and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to give the title compound (7.0 g, 68%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08193351B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-a635430815784b989cdc9500b973476c |
| 出典メモ | uspto-grants-2012_06 |