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HRID 27003作成日:2026年10月24日

4,4'-Bis(dimethylamino)benzophenone → 6,6-Bis(p-dimethylaminophenyl)-6,11-dihydro-[1]benzopyrano[4,3-b]indole

https://huagongshe.com/ja/reaction/27003

反応式

関与物質

役割名称HCID仕込み量
反応物4,4'-Bis(dimethylamino)benzophenoneHCID 7031—
反応物Sodium HydroxideHCID 14798—
反応物Phosphorus oxychlorideHCID 24813—
反応物2-(1H-indol-2-yl)phenolHCID 700009—
溶媒ChloroformHCID 6212—
生成物6,6-Bis(p-dimethylaminophenyl)-6,11-dihydro-[1]benzopyrano[4,3-b]indoleHCID 1263269130.4%

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

DOI10.6084/m9.figshare.5104873.v1
特許番号US04220356
出典データセットuspto-grants-1980_09
ORD IDord-f245225b407842029f8a857b573e11cc
出典メモuspto-grants-1980_09