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HRID 1502463作成日:2026年10月25日

1-Butyl-3-methylimidazolium tetrafluoroborate → HCID 67974760、化合物

https://huagongshe.com/reaction/1502463

反応式

関与物質

役割名称HCID仕込み量
反応物1-Butyl-3-methylimidazolium tetrafluoroborateHCID 2734178—
反応物5-Bromo-4,6-dimethylpyridin-3-amineHCID 7060666—
反応物Nitrilooxonium tetrafluoroborateHCID 11137142—
溶媒Ethyl AcetateHCID 8857—
生成物HCID 67974760HCID 6797476043.3%

反応条件

温度60 °C

反応手順

A mixture of 5-bromo-4,6-dimethyl-pyridin-3-amine (500 mg, 2.49 mmol) and nitrosyl tetrafluoroborate (445 mg, 3.73 mmol) in 1-butyl-3-methylimidazolium tetrafluoroborate (9.48 mL, 49.74 mmol) was heated at 60° C. for 2 hours (caution: exothermic). The reaction mixture was diluted with ethyl acetate (50 mL) and washed with water (2×20 mL), and then saturated aqueous sodium bicarbonate (20 mL). The organic layer was separated, dried over sodium sulfate, filtered and concentrated in vacuo to provide a residue that was purified by flash chromatography (4 g, Silica, 0-50% ethyl acetate in heptane). Desired fractions were combined and evaporated in vacuo to afford the title compound as pale yellow oil (220 mg, 43%), which was used in the next step without further purification.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09206175B2
出典データセットuspto-grants-2015_12
ORD IDord-5d0061673eea48bbb736b6254903156e
出典メモuspto-grants-2015_12