関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Fluoropyridine | HCID 9746 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | (4-[1,3]Dioxolan-2-yl-3-fluoro-phenyl)-methanol | HCID 59255152 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 59255525 | HCID 59255525 | 64.1% |
反応手順
To an N,N-dimethylformamide solution (20 mL) of (4-[1,3]dioxolan-2-yl-3-fluoro-phenyl)-methanol (2.44 g, 12.3 mmol) described in Manufacturing Example 204-1-3 was added sodium hydride (537 mg, 14.8 mmol, 60% in oil), which was cooled to 0° C., after which 2-fluoropyridine (1.27 mL, 14.8 mmol) was added to this suspension, which was stirred for 2 hours at 60° C. The mixture was cooled to room temperature and partitioned into ethyl acetate and water. The organic layer was separated, washed with water, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate:heptane=1:4) to obtain the title compound (2.17 g, 64%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07691882B2 |
|---|
| 出典データセット | uspto-grants-2010_04 |
|---|
| ORD ID | ord-56abc75c59bd42f7b0729e2387481fad |
|---|
| 出典メモ | uspto-grants-2010_04 |
|---|