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HRID 39220作成日:2026年10月24日

Lithium Bromide → 2-Difluoromethoxy-6-nitrobenzonitrile

https://huagongshe.com/ja/reaction/39220

反応式

関与物質

役割名称HCID仕込み量
反応物Lithium BromideHCID 82050—
反応物2-Bromo-1-(difluoromethoxy)-3-nitrobenzeneHCID 58100766—
反応物HCID 178418546HCID 178418546—
溶媒TolueneHCID 1140—
溶媒TetrahydrofuranHCID 8028—
生成物2-Difluoromethoxy-6-nitrobenzonitrileHCID 5810076484.6%

反応条件

温度200 °C

反応手順

A mixture of 2-bromo-1-difluoromethoxy-3-nitro-benzene (1 g, 3.7 mmol), CuCN (0.40 g, 4.5 mmol) and LiBr (0.32 g, 3.7 mmol) in tetrahydrofuran (10 ml) are heated in a microwave oven at 200° C. for 40 minutes. The reaction mixture is cooled to ambient temperature, diluted with toluene and washed with aqueous sodium bromide (1M) and aqueous sodium hydrogen sulfite (saturated). The organic phase is dried over sodium sulfate and concentrated. The residue is purified by HPLC to give 2-difluoromethoxy-6-nitrobenzonitrile (0.67 g, 84% yield). 1H-NMR (CDCl3, 400 MHz): 8.20 (d, 1H), 7.85 (t, 1H), 7.75 (d, 1H), 6.75 (t, 1H) ppm.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08524896B2
出典データセットuspto-grants-2013_09
ORD IDord-47972b48f6ac4d3da12438dc0306f2c1
出典メモuspto-grants-2013_09