関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4,4'-Bis(dimethylamino)benzophenone | HCID 7031 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 2-(1H-indol-2-yl)phenol | HCID 700009 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 6,6-Bis(p-dimethylaminophenyl)-6,11-dihydro-[1]benzopyrano[4,3-b]indole | HCID 12632691 | 30.4% |
反応手順
7.7 g of 4,4'-bisdimethylaminobenzophenone was dissolved in 50 ml of chloroform, and the solution was stirred. Phosphorus oxychloride (5 g) and 10 ml of chloroform were added thereto, and the mixture was stirred for 30 minutes at room temperature (about 20°-30° C.). Then, 6 g of 2-(2'-hydroxyphenyl)indole was added thereto, and the mixture was stirred at room temperature for 3 hours. The mixture was heated under reflux for an additional 2 hours. The heated mixture was cooled to room temperature, and poured into ice water, and neutralized with an aqueous solution of sodium hydroxide. Furthermore, 200 to 300 ml of chloroform was added for extraction. The chloroform layer was washed with water, dried, and distilled under reduced pressure to remove the chloroform. The remaining oily substance was dissolved in a small amount of methanol by heating, and the solution was cooled. The crystals precipitated were separated by filtration, and dried to obtain 4 g of the objective compound having a melting point of 165° to 168° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04220356 |
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| 出典データセット | uspto-grants-1980_09 |
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| ORD ID | ord-f245225b407842029f8a857b573e11cc |
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| 出典メモ | uspto-grants-1980_09 |
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