関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 3-(3-Fluorophenyl)propionic acid | HCID 2737489 | — |
| 反応物 | HCID 68663380 | HCID 68663380 | — |
| 生成物 | HCID 68663808 | HCID 68663808 | 69% |
反応手順
A mixture of 3-[(4-methoxyphenyl)amino]-4-nitrobenzohydrazide (1.60 g, 5.29 mmol), 3-(3-fluorophenyl)propionic acid (0.89 g, 5.29 mmol) and phosphorus oxychloride (5.29 mL) was stirred at 100° C. for 2 hr. The reaction mixture was cooled to 0° C., neutralized with saturated aqueous sodium hydrogen carbonate solution, and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and concentrated. The residue was purified by basic silica gel column chromatography (hexane/ethyl acetate=3/1) to give the title compound (1.51 g, yield 69%) as orange crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08492378B2 |
|---|
| 出典データセット | uspto-grants-2013_07 |
|---|
| ORD ID | ord-0fb9fbefbca142c0bdd18cb622ebc4a1 |
|---|
| 出典メモ | uspto-grants-2013_07 |
|---|