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HRID 240959作成日:2026年10月23日

Ethyl Acetate → 2,3,5-trifluoro-N-(2-fluoro-4-iodophenyl)-6-nitroaniline

https://huagongshe.com/ja/reaction/240959

反応式

関与物質

役割名称HCID仕込み量
反応物Ethyl AcetateHCID 8857—
反応物1,2,3,5-Tetrafluoro-4-nitrobenzeneHCID 67566—
反応物2-Fluoro-4-iodoanilineHCID 185694—
反応物Lithium HexamethyldisilazideHCID 2733832—
溶媒TetrahydrofuranHCID 8028—
生成物2,3,5-trifluoro-N-(2-fluoro-4-iodophenyl)-6-nitroanilineHCID 5743007259.24%

反応条件

温度-78 °C

反応手順

A stirred solution of 2-fluoro-4-iodoaniline (3.64 gm, 15.37 mmol) in dry THF (100 ml) under nitrogen was cooled to −78° C. and a solution of 1.0 M lithium hexa methyl disilazide (LiN(SiMe3)2) “LHMDS” (15.37 ml, 15.37 mmol) was added slowly. This reaction mixture was kept stirring at −78° C. for another hour and then 2,3,4,6-tetrafluoronitrobenzene was added. The reaction mixture was allowed to warm to room temperature and stirring continued for another 16 hours. Ethyl acetate (200 ml) was added to the reaction mixture and was washed with water. Organic layer was dried over sodium sulfate and further purified by column chromatography to provide yellow solid (3.75 gm, yield: 59.24%). M−H+: 410.9. 1H NMR (DMSO, 300 MHz): 6.85 (t, 1H); 7.38 (d, 1H); 7.62 (m, 2H); 8.78 (s, 1H).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08648116B2
出典データセットuspto-grants-2014_02
ORD IDord-d3001c237f7e4fb6a70b29de9dd72c68
出典メモuspto-grants-2014_02