関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,4-Dichloro-5-methoxyaniline | HCID 1476636 | — |
| 反応物 | Pyridinium chloride | HCID 10176127 | — |
| 反応物 | HCID 178486400 | HCID 178486400 | — |
| 溶媒 | Glycol monoethyl ether | HCID 8076 | — |
| 溶媒 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | HCID 178486403 | HCID 178486403 | 65.6% |
反応手順
A mixture of 0.7 g (2.46 mmol) of 4-chloro-8-hydroxy-7-methoxybenzo[g]quinoline-3-carbonitrile, 0.57 g (2.95 mmol) of 2,4-dichloro-5-methoxyaniline and 0.28 g (2.46 mmol) of pyridine hydrochloride in 7 mL of 2-ethoxyethanol is heated at 120° C. for 2 hours, then cooled to room temperature. The product mixture is diluted with saturated solution of sodium bicarbonate and stirred for 15 minutes. The resulting solid is collected by filtration, washed with water and dried. The crude product is purified by silica gel chromatography, utilizing a 98:2 to 90:10 gradient of methylene chloride/methanol to give 0.71 g of 4-(2,4-dichloro-5-methoxyphenylamino)-8-hydroxy-7-methoxybenzo[g]quinoline-3-carbonitrile as a yellow solid, mp, 238-240° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06638929B2 |
|---|
| 出典データセット | uspto-grants-2003_10 |
|---|
| ORD ID | ord-e2d580160bfb4dcea4b7e35feca411e0 |
|---|
| 出典メモ | uspto-grants-2003_10 |
|---|