関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | P-Anisidine | HCID 7732 | — |
| 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 | 4-Pyridinecarboxylic acid, 3-[(4-methoxyphenyl)amino]- | HCID 618471 | 13% |
反応手順
3-Fluoro-isonicotinic acid (50 mg, 0.354 mmol) and p-anisidine (44 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 RP chromatography to give 11 mg (45 μmol; 13% yield) of pure desired product. LC-MS (method V): rt=1.82 min; m/z [M+H]+ 245.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08524911B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
|---|
| ORD ID | ord-cdf9d91d0a3f413cb5c8964d06b2c0c7 |
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| 出典メモ | uspto-grants-2013_09 |
|---|
