関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 4-Fluorophenylhydrazine hydrochloride | HCID 69981 | — |
| 反応物 | 2-(Fluoromethoxy)benzaldehyde | HCID 20061507 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 1-(4-Fluorophenyl)-5-methoxy-1H-indazole | HCID 59339622 | — |
反応手順
A mixture of 2-fluoromethoxybenzaldehyde (2.1 mmol, 320 mg), 4-fluorophenylhydrazine hydrochloride (2.1 mmol, 340 mg) and cesium carbonate (3 mmol, 2.0 g) in NMP (6 ml) was heated in a microwave reactor (300 W, 20 min, 150° C.). After cooling to r.t. the reaction mixture was diluted with dichloromethane (20 ml) and washed with 1M HCl, and sat. NaHCO3. The organic layer was dried over Na2SO4, concentrated, and purified by flash chromatography on silica gel (heptane-ethyl acetate).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07728030B2 |
|---|
| 出典データセット | uspto-grants-2010_06 |
|---|
| ORD ID | ord-c8e87cd6e7c044e2b1f536b44b2227db |
|---|
| 出典メモ | uspto-grants-2010_06 |
|---|
