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HRID 594846作成日:2026年10月26日

Cesium carbonate → Di-tert-butyl {6'-[(3-methoxypyridin-2-yl)amino]dispiro[1,3-oxazole-4,4'-chromene-3',3''-oxetan]-2-yl}imidodicarbonate

https://huagongshe.com/reaction/594846

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1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 636044—
反応物2-Amino-3-methoxypyridineHCID 9920384—
反応物Di-tert-butyl (6'-bromodispiro[1,3-oxazole-4,4'-chromene-3',3''-oxetan]-2-yl)imidodicarbonateHCID 86724239—
触媒Bis(dibenzylideneacetone)palladiumHCID 9811564—
溶媒1,4-DioxaneHCID 31275—
生成物Di-tert-butyl {6'-[(3-methoxypyridin-2-yl)amino]dispiro[1,3-oxazole-4,4'-chromene-3',3''-oxetan]-2-yl}imidodicarbonateHCID 86724238—

反応条件

温度100 °C

反応手順

A mixture of di-tert-butyl (6′-bromodispiro[1,3-oxazole-4,4′-chromene-3′,3″-oxetan]-2-yl)imidodicarbonate (300 mg, 0.571 mmol), 3-methoxypyridin-2-amine (354 mg, 2.86 mmol), tris(dibenzylideneacetone)dipalladium(0) (105 mg, 0.114 mmol), (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (198 mg, 0.343 mmol), Cs2CO3 (558 mg, 1.71 mmol) and dioxane (15 mL) was stirred for 48 hours at 100° C. The reaction mixture was cooled down to ambient temperature, and partitioned with CHCl3 and water. The organic layer was dried over Na2SO4, and filtered. The filtrate was concentrated at reduced pressure, to give crude di-tert-butyl {6′-[(3-methoxypyridin-2-yl)amino]dispiro[1,3-oxazole-4,4′-chromene-3′,3″-oxetan]-2-yl}imidodicarbonate, which was used for the next reaction without further purification.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09242973B2
出典データセットuspto-grants-2016_01
ORD IDord-553cf72ccbb04e97a70f38172fc4878d
出典メモuspto-grants-2016_01