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HRID 34004作成日:2026年10月23日

Diisopropylamine → (3-Fluorophenyl)-(3-fluoropyridin-4-yl)-methanol

https://huagongshe.com/ja/reaction/34004

反応式

関与物質

役割名称HCID仕込み量
反応物DiisopropylamineHCID 7912—
反応物Ammonium ChlorideHCID 25517—
反応物3-FluoropyridineHCID 67794—
反応物3-FluorobenzaldehydeHCID 68009—
反応物ButyllithiumHCID 178418339—
溶媒TetrahydrofuranHCID 8028—
溶媒HexaneHCID 8058—
溶媒Ethyl AcetateHCID 8857—
生成物(3-Fluorophenyl)-(3-fluoropyridin-4-yl)-methanolHCID 23070104—

反応条件

温度0 °C

反応手順

Under nitrogen atmosphere, a solution of 6.1 mL of diisopropylamine in 100 ml of dehydrated tetrahydrofuran was cooled to −70° C., added with 28 mL of 1.56 M n-butyllithium in hexane, and stirred at 0° C. for 15 minutes. After cooling to −70° C., 3.4 mL of 3-fluoropyridine was added dropwise, stirred at the same temperature for 4 hours, and then added dropwise with 4.8 mL of 3-fluorobenzaldehyde. After stirring for 1 hour, aqueous ammonium chloride and ethyl acetate were successively added, and the reaction solution was recovered to room temperature. The organic layer was extracted, washed with water, and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the resulting residue was recrystallized from diisopropyl ether, to afford 7.1 g of the title compound as colorless cubic crystals.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07429609B2
出典データセットuspto-grants-2008_09
ORD IDord-d9e6388343e342d9824144a604857359
出典メモuspto-grants-2008_09