関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-((Trifluoromethyl)thio)aniline | HCID 123054 | — |
| 反応物 | 3-Fluoropyridine-4-carboxylic acid | HCID 345361 | — |
| 反応物 | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-(4-Trifluoromethylsulfanyl-phenylamino)-isonicotinic acid | HCID 57649642 | 10% |
反応手順
3-Fluoro-isonicotinic acid (50 mg, 0.354 mmol) and 4-(trifluoromethylthio)aniline (68.5 mg, 0.354 mmol) was added to 2 ml dry THF and the mixture was cooled to −78° C. LiHMDS (1M in THF, 1.24 ml) was added and the mixture was allowed to warm to room temperature over night. Hydrochloric acid (1M in methanol, 5 ml) was added and the volatiles were removed in vacuo. The crude material was purified by preparative HPLC to give 11.4 mg (45 μmol; 10% yield) of pure desired product. LC-MS (method V): rt=3.09 min; m/z [M+H]+ 315.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07956191B2 |
|---|
| 出典データセット | uspto-grants-2011_06 |
|---|
| ORD ID | ord-6de2c2f04d604cc4bc7363cb54b357aa |
|---|
| 出典メモ | uspto-grants-2011_06 |
|---|
