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HRID 62073作成日:2026年10月23日

3,5-Dimethylaniline → 1-(3,5-dimethylphenyl)-3-(3-(4-(1-(4-(trifluoromethoxy)phenyl)-1H-1,2,4-triazol-3-yl)phenyl)propyl)urea

https://huagongshe.com/ja/reaction/62073

反応式

関与物質

役割名称HCID仕込み量
反応物3,5-DimethylanilineHCID 7949—
反応物Cesium carbonateHCID 10796—
反応物TriphosgeneHCID 94429—
反応物IsocyanateHCID 105034—
反応物Sodium BicarbonateHCID 516892—
反応物3-(4-(1-(4-(trifluoromethoxy)phenyl)-1H-1,2,4-triazol-3-yl)phenyl)propan-1-amineHCID 90404268—
溶媒DichloromethaneHCID 6344—
生成物1-(3,5-dimethylphenyl)-3-(3-(4-(1-(4-(trifluoromethoxy)phenyl)-1H-1,2,4-triazol-3-yl)phenyl)propyl)ureaHCID 118675054—

反応手順

To 3-(4-(1-(4-(trifluoromethoxy)phenyl)-1H-1,2,4-triazol-3-yl)phenyl)propan-1-amine (1 equiv) and sodium bicarbonate (5 equiv) in an appropriate reaction vessel may be added a solvent such as dichloromethane (at a concentration between about 0.01 M to about 1 M). The reaction may be placed in an ice bath and triphosgene (0.4 equiv) can be added in one portion. The reaction may be monitored by LC/MS to observe formation of the isocyanate, upon which the reaction may be diluted with dichloromethane, filtered through a phase separator, and concentrated. The residue may be suspended in a solvent such as acetonitrile (0.1 M to about 1 M), followed by addition of 3,5-dimethylaniline (1.0-1.5 equiv) and cesium carbonate (1.0-1.5 equiv). Following completion of the reaction, the product may be obtained using standard organic chemistry techniques of workup and purification.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09445594B2
出典データセットuspto-grants-2016_09
ORD IDord-9350c550cd144124824bfd8f59bdfe70
出典メモuspto-grants-2016_09