関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 6-Fluoro-2-methyl-3-nitropyridine | HCID 12408185 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 4-(6-Methyl-5-nitro-2-pyridinyl)morpholine | HCID 8208955 | 99% |
反応手順
To a solution of 2-fluoro-5-nitro-6-picoline (3.0 g, 19.2 mmol) in DMSO (26 mL) were added morpholine (3.35 mL, 38.4 mmol) and potassium carbonate (6.64 g, 48.0 mmol). The reaction mixture was allowed to stir overnight, at 70° C. The reaction mixture was then partitioned between EtOAc (40 mL) and water (40 mL). The organic solution was separated and the aqueous solution was extracted with EtOAc (2×40 mL). The organic solutions were combined, washed with brine, dried over MgSO4, filtered and concentrated to give 4-(6-methyl-5-nitropyridin-2-yl) morpholine (4.0 g, 99%), as a muddy green solid. LCMS (FA): Rt=1.59 min, m/z=224.0 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08507667B2 |
|---|
| 出典データセット | uspto-grants-2013_08 |
|---|
| ORD ID | ord-21c7a97b69c04ff18d8c1990e7d48885 |
|---|
| 出典メモ | uspto-grants-2013_08 |
|---|