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HRID 1018176作成日:2026年10月23日

Ammonia → 4-Amino-3,5-dichlorobenzotrifluoride

https://huagongshe.com/ja/reaction/1018176

反応式

関与物質

役割名称HCID仕込み量
反応物AmmoniaHCID 222—
反応物Lithium fluorideHCID 224478—
反応物1,2,3-Trichloro-5-(trifluoromethyl)benzeneHCID 2733399—
溶媒N-methyl-2-pyrrolidoneHCID 13387—
生成物4-Amino-3,5-dichlorobenzotrifluorideHCID 14109472.2%

反応条件

温度-95 °C

反応手順

3,4,5-Trichloro-trifluoromethylbenzene (0.681 g, 2.73 mmol), lithium fluoride (7.1 mg, 0.273 mmol) and N-methylpyrrolidone (1.8 ml) are mixed in an autoclave. The autoclave is cooled to −95° C. and then ammonia (1.3 g, 76.4 mmol) is added. The autoclave is then heated at 250° C. and with stirring for 4 h and is subsequently allowed to return to room temperature. The reaction product is extracted by washing with water and with dichloromethane and then the organic phase is evaporated, after having been dried. 0.453 g (1.97 mmol) of 2,6-dichloro-4-trifluoromethylaniline is obtained with a degree of conversion of the 3,4,5-trichloro-trifluoromethylbenzene of 97%, a ratio equal to 83/17 for the selectivity for 2,6-dlchloro-para-trifluoromethylaniline with respect to 2,6-dichloro-meta-trifluoromethylaniline and an 87% yield of 2,6-dichloro-para-trifluoromethylaniline.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06479703B1
出典データセットuspto-grants-2002_11
ORD IDord-6475831cd98b4b2986b7ef106e72a8e5
出典メモuspto-grants-2002_11