化工社化工社 化学情報印刷レポート · 研究参考用
Naphthalic anhydride → 8-(6-Ethylamino-3-ethylimino-2,7-dimethyl-3H-xanthen-9-yl)naphthalene-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Naphthalic anhydride | HCID 6693 | — |
| 反応物 | 3-Ethylamino-4-methylphenol | HCID 8428 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 8-(6-Ethylamino-3-ethylimino-2,7-dimethyl-3H-xanthen-9-yl)naphthalene-carboxylic acid | HCID 21988382 | 10.8% |
反応手順
3-Ethylamino-4-methyl-phenol (0.3 g, 2 mmol) and benzo[de]isochromene-1,3-dione (0.2 g, 1 mmol) in sulfuric acid (3 ml) was heated to 150° C. over a period of 6 h. The reaction mixture was pouring into crushed ice, allowed to stand over a period of 1 h and the precipitate was filtered. The filtrate was neutralized with concentrated ammonium hydroxide and concentrated to give a dark purple residue. Purification via preparatory layer chromatography (PLC, 1 mm silica gel, 9/1 DCM: MeOH, 2% AcOH) gave the title compound (50 mg). ABS λmax=527 nm (EtOH).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07091348B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-d406d35cc3c140e4a123a0c440055f56 |
| 出典メモ | uspto-grants-2006_08 |