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HRID 384131作成日:2026年10月26日

Sodium Carbonate → HCID 178515654、化合物

https://huagongshe.com/reaction/384131

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium CarbonateHCID 10340—
反応物4-Fluorophenylboronic acidHCID 285645—
反応物HCID 178515655HCID 178515655—
溶媒DME dimethoxyethaneHCID 22508344—
生成物HCID 178515654HCID 178515654—

反応条件

温度90 °C

反応手順

To a solution of 5-(4-(2-(6-chloropyridin-2-yl)ethoxy)phenyl)isoxazol-3-ol (46.5 mg) in dimethoxyethane ethylene glycol dimethyl ether (3 ml), 18 mg of tetrakis triphenylphosphine palladium, 31 mg of 4-fluorophenylboronic acid and 0.2 ml of 2M aqueous sodium carbonate solution were added, and the reaction solution was stirred at 90° C. for 2 hours. The reaction solution was cooled, then diluted with a saturated saline solution, extracted with ethyl acetate, and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue obtained was purified through reversed phase medium pressure liquid chromatography (ODS-AS-360-CC (by YMC), mobile phase: water-acetonitrile-0.1% trifluoroacetic acid). The solvent of the resultant fraction was diluted with ethyl acetate, washed with saturated sodium bicarbonate water, and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue obtained was purified by preparative thin layer chromatography (Kieselgel™ 60 F254, Art5744, made by Merck & Co., methanol/chloroform (1:9)) to afford the title compound as a brown solid.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08367708B2
出典データセットuspto-grants-2013_02
ORD IDord-d0326201dd334b81a4ca02e7f930a220
出典メモuspto-grants-2013_02