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HRID 331690作成日:2026年10月26日

Triethylamine → 1-Chloro-4-{1-[(E)-2-nitroethenyl]cyclobutyl}benzene

https://huagongshe.com/reaction/331690

反応式

関与物質

役割名称HCID仕込み量
反応物TriethylamineHCID 8471—
反応物Trifluoroacetic anhydrideHCID 9845—
反応物1-(1-(4-Chlorophenyl)cyclobutyl)-2-nitroethanolHCID 66747669—
溶媒DichloromethaneHCID 6344—
生成物1-Chloro-4-{1-[(E)-2-nitroethenyl]cyclobutyl}benzeneHCID 66746852—

反応条件

温度0 °C

反応手順

1-(1-(4-Chlorophenyl)cyclobutyl)-2-nitroethanol (5.2 g, 20.34 mmol) was dissolved in dichloromethane (41 ml) and trifluoroacetic acid anhydride (2.87 ml, 20.34 mmol) was added. The reaction mixture was cooled to 0° C. and triethylamine (5.67 ml, 40.7 mmol) was added dropwise. The reaction was slowly warmed to room temperature and stirring Was continued for 2 h. The reaction mixture was diluted with dichloromethane and washed with aqueous hydrochloric acid (1 N). The organic layer was dried (magnesium sulfate) and concentrated in vacuo. The crude product was purified by flash chromatography (silica, dichloromethane, methanol). Yield: 3.99 g (16.79 mmol, 83%)

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08877794B2
出典データセットuspto-grants-2014_11
ORD IDord-0d12ee125a564d98892a285f8e239deb
出典メモuspto-grants-2014_11