関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cyclobutylamine | HCID 75645 | — |
| 反応物 | 3-Bromo-5-fluoropyridine | HCID 820206 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 5-bromo-N-cyclobutylpyridin-3-amine | HCID 59619987 | — |
反応手順
A mixture of 3-bromo-5-fluoropyridine (Frontier Scientific, Logan, USA, 5.63 mmol) and cyclobutylamine (Fluka, Buchs, Switzerland, 12.38 mmol) in NMP (8 ml) was heated under microwave irradiation for 1 h at 190° C. and for 5.5 h at 200° C. The reaction mixture was diluted with EtOAc and washed with saturated aqueous NaHCO3, with brine (3×), dried over Na2SO4, filtered, evaporated and dried under vacuum to give the title compound as an off-white solid. (HPLC: tR 2.31 min (Method A); M+H=227, 229 MS-ES)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08476294B2 |
|---|
| 出典データセット | uspto-grants-2013_07 |
|---|
| ORD ID | ord-1c537545f2964122a62d2fd303c60f36 |
|---|
| 出典メモ | uspto-grants-2013_07 |
|---|
