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HRID 384235作成日:2026年10月25日

Triethylamine → HCID 66899075、化合物

https://huagongshe.com/reaction/384235

反応式

関与物質

役割名称HCID仕込み量
反応物TriethylamineHCID 8471—
反応物DiphosgeneHCID 10426—
反応物2-Fluoro-4-(trifluoromethyl)anilineHCID 2737674—
反応物3-Amino-5-fluorobenzonitrileHCID 2756432—
溶媒WaterHCID 962—
溶媒TetrahydrofuranHCID 8028—
生成物HCID 66899075HCID 6689907583.9%

反応手順

A solution of 6.15 g (45.18 mmol) of 5-fluoro-3-cyanoaniline in 90 ml of tetrahydrofuran is stirred at ambient temperature under an argon atmosphere. 4.3 ml (36.14 mmol) of diphosgene are added dropwise then 30 ml (135.54 mmol) of triethylamine. After refluxing in the reaction mixture for 3 hours, a solution of 7.10 g (39.64 mmol) of 4-amino-3-fluorotrifluoromethylbenzene in 10 ml of tetrahydrofuran is slowly added. The reflux is maintained for an additional 2 hours. The medium is then stirred into 100 ml of water, then extracted with 100 ml of ethyl acetate. The organic phase is washed with 100 ml of a saturated sodium chloride solution, dried over magnesium sulphate and concentrated to dryness using a rotary evaporator. The solid residue obtained is recrystallized at high temperature in 90 ml of acetonitrile in order to give 10.35 g of 1-(2-fluoro-4-trifluoromethylphenyl)-3-(3-cyano-5-fluorophenyl)urea in the form of a cream solid.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08367715B2
出典データセットuspto-grants-2013_02
ORD IDord-0f50632ec1d1498c9434864b5c0910d8
出典メモuspto-grants-2013_02