化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → Benzoic acid, 2-[(2-bromophenyl)thio]-5-nitro-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 2-Bromobenzenethiol | HCID 80598 | — |
| 反応物 | 2-Fluoro-5-nitrobenzoic acid | HCID 280997 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Benzoic acid, 2-[(2-bromophenyl)thio]-5-nitro- | HCID 43090919 | 99% |
反応手順
2-Bromobenzenethiol (7.2 ml, 85.9 mmol) was added to a solution of KOH (9.6 g, 172 mmol) in water (50 ml) degassed for 15 minutes. 2-Fluoro-5-nitrobenzoic acid (15.9 g, 85.9 mmol) was added to the reaction mixture, which was refluxed under a nitrogen atmosphere overnight. The reaction was cooled to room temperature and was acidified (pH 1) with conc. HCl. The precipitate formed was filtered and dried overnight in a vacuum oven (50° C.) to give the crude title compound as a pale yellow solid (30 g, 99%). The product was used without further purification. m/z (LC-MS, ESP), RT=4.51min, (M−−1)=352-354, (1:1, bromine isotope ratio present).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07429660B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-d76cec926c5e4cbd8ab02ae004f84f9b |
| 出典メモ | uspto-grants-2008_09 |