化工社化工社 化学情報印刷レポート · 研究参考用
Carbon Dioxide → Benzoic acid, 2-(methylthio)-4-(trifluoromethyl)-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Carbon Dioxide | HCID 280 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Benzene, 1-bromo-2-(methylthio)-4-(trifluoromethyl)- | HCID 11000144 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Benzoic acid, 2-(methylthio)-4-(trifluoromethyl)- | HCID 11085762 | — |
反応手順
n-Butyllithium (2.5M in hexane, 25 ml) was added under an inert atmosphere to a stirred solution of 4-bromo-3-(methylsulphenyl)benzotrifluoride (16.4 g) in ether maintaining the temperature below -70° C. for 2 hours. The mixture was poured onto solid carbon dioxide pellets, stirred for 10 rains and aqueous hydrochloric acid added. The layers were separated and the aqueous layer was extracted with ether. The combined organic layers were washed with water, dried (MgSO4) and filtered. The filtrate was evaporated and the residue was triturated with cyclohexane and filtered to give 2-(methylsulphenyl)-4-trifluoromethylbenzoic acid (12.4 g) as a white solid NMR (CDCl3 +DMSO-d6): 2.45 (s,3H), 7.2(d,1H), 7.3(s,1H), 8.0(d,1H), 10.7-11(bs,1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05424276 |
| 出典データセット | uspto-grants-1995_06 |
| ORD ID | ord-4b763ab9c11f46fdbe59706e9ea487f7 |
| 出典メモ | uspto-grants-1995_06 |