関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 反応物 | Methyl 3-amino-6-(2,6-difluorophenyl)-5-fluoropicolinate | HCID 59226608 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Amino-6-(2,6-difluorophenyl)-5-fluoropicolinic acid | HCID 59226513 | 86% |
反応手順
To a mixture of methyl 3-amino-6-(2,6-difluorophenyl)-5-fluoropyridine-2-carboxylate (84.0 mg, 0.298 mmol) and lithium hydroxide, monohydrate (40.2 mg, 0.958 mmol), THF (2.0 mL) was added followed by water (1.0 mL). The mixture was heated at 50° C. for 3 h. The reaction was then cooled to 0° C. for, and 1 M HCl was added slowly until the pH reached 2. The reaction mixture was then diluted with water (20 mL), extracted with EtOAc (3×20 mL), and the combined organic extract was washed with brine (30 mL), dried over Na2SO4, and concentrated under reduced pressure to give the sub-title compound as a white solid (68.5 mg, 86%). LCMS calc. for C12H8F3N2O2 (M+H)+: m/z=269.0. found 269.0.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09200004B2 |
|---|
| 出典データセット | uspto-grants-2015_12 |
|---|
| ORD ID | ord-72612c69293f44c0a25b7c8d56717e01 |
|---|
| 出典メモ | uspto-grants-2015_12 |
|---|