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HRID 873700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/873700

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US08975415B2
出典データセットuspto-grants-2015_03
ORD IDord-8168d583c1fc4a36b941a44fc62f8107
出典メモuspto-grants-2015_03