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HRID 612005作成日:2026年10月25日

Water → 8-(3-Bromophenylamino)[1,3]dioxolo[4,5-g]quinoline-7-carbonitrile

https://huagongshe.com/reaction/612005

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物BromochloromethaneHCID 6333—
反応物Cesium carbonateHCID 10796—
反応物4-(3-Bromophenylamino)-6,7-dihydroxy-3-quinolinecarbonitrileHCID 135402848—
溶媒DimethylformamideHCID 6228—
生成物8-(3-Bromophenylamino)[1,3]dioxolo[4,5-g]quinoline-7-carbonitrileHCID 532888342.4%

反応条件

温度111 °C

反応手順

A mixture of 2.17 g (6.09 mmole) of 4-[(3-bromophenyl)amino]-6,7-dihydroxy-3-quinolinecarbonitrile, 0.59 ml (1.18 g; 9.14 mmole) of bromochloromethane and 2.98 g (9.14 mmole) of cesium carbonate in 20 ml of N,N-dimethylformamide was heated and stirred for 2 hours in an oil bath at 111° C. The reaction was poured into 75 ml of water and extracted with four 50 ml portions of methylene chloride. The combined methylene chloride extracts were washed with several portions of water. This solution was taken to an oil in vacuo and this was dissolved in ethyl acetate. This solution was washed repeatedly with water, then with brine. The solution was dried over anhydrous magnesium sulfate, and taken to a solid in vacuo to give 0.95 g of 8-[(3-bromophenyl)amino]-[1,3]-dioxolo[4,5-g]quinoline-7-carbonitrile, m.p. 201-205° C.: mass spectrum (electrospray, m/e): M+H 368.1, 370.1.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06002008
出典データセットuspto-grants-1999_12
ORD IDord-cdb09c24625442dba30f7c3bc7768128
出典メモuspto-grants-1999_12