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3-Amino-5-fluorobenzonitrile → 1-(2-Chloro-4-trifluoromethylphenyl)-3-(3-cyano-5-fluorophenyl)urea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Amino-5-fluorobenzonitrile | HCID 2756432 | — |
| 反応物 | 2-Chloro-4-(trifluoromethyl)phenyl isocyanate | HCID 5102533 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-(2-Chloro-4-trifluoromethylphenyl)-3-(3-cyano-5-fluorophenyl)urea | HCID 66898760 | 84.4% |
反応手順
A solution of 15 g (110.2 mmol) of 5-fluoro-3-cyanoaniline in 150 ml of tetrahydrofuran is stirred at ambient temperature under an argon atmosphere. Next, 17.5 ml (121.22 mmol) of 2-chloro-4-trifluoromethylphenylisocyanate are added. The reaction medium is heated at reflux for 3 hours then concentrated to dryness using a rotary evaporator. The solid residue obtained is recrystallized at high temperature in 60 ml of ethyl acetate in order to give 33.25 g of 1-(2-chloro-4-trifluoromethylphenyl)-3-(3-cyano-5-fluorophenyl)urea in the form of a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08367715B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-994db13d8f6741d181374bec16f2100a |
| 出典メモ | uspto-grants-2013_02 |