化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 5-[(2-Chloro-alpha,alpha,alpha-trifluoro-p-tolyl)oxy]salicylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2,5-Dihydroxybenzoic acid | HCID 3469 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Benzene, 2-chloro-1-fluoro-4-(trifluoromethyl)- | HCID 157153 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-[(2-Chloro-alpha,alpha,alpha-trifluoro-p-tolyl)oxy]salicylic acid | HCID 86750233 | 91.3% |
反応手順
A mixture of 3-chloro-4-fluoro-α,α,α-trifluorotoluene (103 g, 0.52 mol), 2,5-dihydroxybenzoic acid (80 g, 0.52 mol) and potassium carbonate (180 g, 1.3 mol) in dimethyl sulfoxide is heated to and held at 130° C. for about 30 hours, cooled to room temperature and poured into ice-water. The aqueous mixture is acidified to pH 2 with concentrated hydrochloric acid and decanted to obtain an oil. The oil is dissolved in methylene chloride, washed with water and concentrated in vacuo to form a brown oil which is crystallized from ether to give the title product as a tan solid (158 g, 91.3%, mp 135° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05596124 |
| 出典データセット | uspto-grants-1997_01 |
| ORD ID | ord-43534e15d35d4e928e8f2f3a64764d6f |
| 出典メモ | uspto-grants-1997_01 |