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HRID 70526作成日:2026年10月25日

Cesium carbonate → (2E)-3-(4-tert-Butylphenyl)-3-(5-chloro-6-methoxypyridin-2-yl)prop-2-en-1-ol

https://huagongshe.com/reaction/70526

反応式

関与物質

役割名称HCID仕込み量
反応物Cesium carbonateHCID 10796—
反応物Tris(furan-2-yl)phosphaneHCID 521585—
反応物4-tert-Butylphenylboronic acidHCID 2734320—
反応物(2Z)-3-(5-Chloro-6-methoxypyridin-2-yl)-3-iodoprop-2-en-1-olHCID 58452855—
触媒Bis(dibenzylideneacetone)palladiumHCID 9811564—
溶媒WaterHCID 962—
溶媒Ethyl AcetateHCID 8857—
溶媒1,4-DioxaneHCID 31275—
生成物(2E)-3-(4-tert-Butylphenyl)-3-(5-chloro-6-methoxypyridin-2-yl)prop-2-en-1-olHCID 58452849101.6%

反応条件

温度65 °C

反応手順

4-tert-Butylphenylboronic acid (3.5 g), tris(dibenzylideneacetone)dipalladium(0) (183 mg), tri(2-furyl)phosphine (280 mg) and cesium carbonate (1.98 g) were added to a solution of (2Z)-3-(5-chloro-6-methoxypyridin-2-yl)-3-iodoprop-2-en-1-ol (881 mg) in 1,4-dioxane (20 mL)-water (10 mL) in a nitrogen atmosphere, and the mixture was stirred at an external temperature of 65° C. for 1.5 hours. The reaction solution was left to cool, diluted with ethyl acetate and filtered. The filtrate was washed with brine and dried over sodium sulfate. After filtration, the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=19:1→1:1) to give the title compound as a light yellow powder (912 mg, 91%).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08822503B2
出典データセットuspto-grants-2014_09
ORD IDord-08a57a96d9184121a1cb0aadff6dac11
出典メモuspto-grants-2014_09