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Hydrochloric Acid → 2-Chloro-5-sulfino-benzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Sodium Sulfite | HCID 24437 | — |
| 反応物 | 2-Chloro-5-(fluorosulpho)benzoic acid | HCID 88873 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Chloro-5-sulfino-benzoic acid | HCID 15112904 | 76.5% |
反応手順
A solution of 33.59 g (267 mmol) sodium sulfite in 100 ml water at 0° C. is treated with 21.2 g (89 mmol) 2-Chloro-5-fluorosulfonyl-benzoic acid and 26.6 ml of a 10M aqueous NaOH solution (267 mmol). The mixture was allowed to stirr for 3 h at room temperature, acidified with HCl conc. (pH=4) and water was removed under vacuum. Methanol was added, the precipitate filtered off and the filtrate concentrated. Methanol and diethylether were added and the precipitate was filtered off washed with ether and dried to yield 15 g (76.5%) of the title compound as white gum. MS (m/e): 219.1 (MH−, 100%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07427612B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-ddda5ef23f3d423d8332ec0fccf56639 |
| 出典メモ | uspto-grants-2008_09 |