Sodium Carbonate → 1-((4'-Butoxy(1,1'-biphenyl)-4-yl)thio)-3-(4,4-dimethyl-2,5-dioxoimidazolidin-1-yl)-2-propanone

https://huagongshe.com/reaction/1978025

関与物質

役割	名称	HCID	仕込み量
反応物	Sodium Carbonate	HCID 10340	—
反応物	4-Butoxyphenylboronic Acid	HCID 3836310	—
反応物	1-(4-Bromophenylthio)-3-(4,4-dimethyl-2,5-dioxoimidazolidin-1-yl)-2-propanone	HCID 21700262	—
触媒	Tetrakis(triphenylphosphine)palladium	HCID 11979704	—
溶媒	1,2-Dimethoxyethane	HCID 8071	—
溶媒	Ethyl Acetate	HCID 8857	—
生成物	1-((4'-Butoxy(1,1'-biphenyl)-4-yl)thio)-3-(4,4-dimethyl-2,5-dioxoimidazolidin-1-yl)-2-propanone	HCID 11037553	78.1%

反応条件

温度	90 °C

反応手順

A solution of Example 46A (700 mg, 1.89 mmol) in DME (20 mL) at room temperature was treated with 4-n-butoxybenzeneboronic acid (549 mg, 2.83 mmol), tetrakis-(triphenylphosphine)-palladium (218 mg, 0.189 mmol) and 1M sodium carbonate (3.54 mL, 3.54 mmol), the reaction vessel was sealed and heated at 90° C. for 6 hours, diluted with ethyl acetate, washed with sequentially saturated ammonium chloride solution, water and brine, dried (Na2SO4), filtered, concentrated and purified on silica gel with 30 to 50% ethyl acetate/dichloromethane to provide 650 mg (78%) of the desired product as a yellow solid.

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US06235786B1
出典データセット	uspto-grants-2001_05
ORD ID	ord-89b45d9ae1264a8bb277584400006a80
出典メモ	uspto-grants-2001_05