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Sulfamic Acid → 5-Methoxy-2-nitrobenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfamic Acid | HCID 5987 | — |
| 反応物 | 5-Methoxy-2-nitrobenzaldehyde | HCID 230371 | — |
| 反応物 | Propan-2-one--water (1/1) | HCID 18366337 | — |
| 反応物 | Sodium Chlorite | HCID 23668197 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-Methoxy-2-nitrobenzoic acid | HCID 339209 | — |
反応手順
Sulfamic acid (15.73 g, 0.162 mol) is added to a solution of 5-methoxy-2-nitrobezaldehyde (19.6 g, 0.108 mol) in an acetone/water (1:1) mixture. Sodium chlorite (18.31 g, 80% real, 0.162 mol) is then added to the reaction mixture at a rate which maintains the reaction mixture temperature below 40° C. The resultant reaction mixture is stirred at room temperature for 24 hours and poured into water. The aqueous mixture is extracted with ethyl acetate. The organic extracts are combined, washed sequentially with 2N hydrochloric acid and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to give the title product as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05519133 |
| 出典データセット | uspto-grants-1996_05 |
| ORD ID | ord-fe3a904c9bd64944ba14beadcb52ad44 |
| 出典メモ | uspto-grants-1996_05 |