関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 6-Bromopyridine-2-carboxylic acid | HCID 593919 | — |
| 溶媒 | Thionyl Chloride | HCID 24386 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 6-Bromopyridine-2-carboxamide | HCID 21961408 | 45% |
反応手順
6-Bromopicolinic acid (1000 mg, 4.95 mmol) was suspended in thionyl chloride (15 mL) and heated at 70° C. for 5 h. The reaction was cooled to room temperature and the volatiles were condensed under reduced pressure. A solution of ammonia (2M in dioxane (15 mL) was added to the residue and then the solvents were removed under reduced pressure. The crude residue was purified by MPLC with a gradient of 0 to 20% MeOH/dichloromethane to give 6-Bromo-pyridine-2-carboxylic acid amide as a white powder (555 mg, 45%). MS ES (MH+=201.0/203.0).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07659412B2 |
|---|
| 出典データセット | uspto-grants-2010_02 |
|---|
| ORD ID | ord-a8e0a4f17b6945e3abad1fe4c1b799e3 |
|---|
| 出典メモ | uspto-grants-2010_02 |
|---|
