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HRID 1377637作成日:2026年10月27日

Piperidine → 5-[4-[4-[2-(5-Methyl-2-phenyl-4-oxazolyl)ethoxy]phenyl]butylidene]-2,4-oxazolidinedione

https://huagongshe.com/reaction/1377637

反応式

関与物質

役割名称HCID仕込み量
反応物PiperidineHCID 8082—
反応物2,4-OxazolidinedioneHCID 97389—
反応物2-[3-[4-[2-(5-Methyl-2-phenyl-4-oxazolyl)ethoxy]phenyl]propyl]-1,3-dioxaneHCID 11025902—
溶媒Acetic AcidHCID 176—
生成物5-[4-[4-[2-(5-Methyl-2-phenyl-4-oxazolyl)ethoxy]phenyl]butylidene]-2,4-oxazolidinedioneHCID 5703161026%

反応手順

A mixture of 2-[3-[4-[2-(5-methyl-2-phenyl-4-oxazolyl)ethoxy]phenyl]propyl]-1,3-dioxane (2.0 g), 2,4-oxazolidinedione (0.99 g), piperidine (0.21 g) and acetic acid (50 ml) was heated for 24 hours under reflux. The reaction mixture was concentrated under reduced pressure, to which was added ethyl acetate. The ethyl acetate layer was washed with an aqueous solution of sodium hydrogencarbonate, 2N HCl and water, successively, which was then dried (MgSO4), followed by concentration. The concentrate was purified by means of a silica gel column chromatography. From the fractions eluted with chloroform--ethyl acetate (5:1), 5-[4-[4-[2-(5-methyl-2-phenyl-4-oxazolyl)ethoxy]phenyl]butylidene]-2,4-oxazolidinedione (0.55 g, 26%) was obtained. Recrystallization from ethyl ether - methanol gave colorless needles, m.p.152°-153° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05665748
出典データセットuspto-grants-1997_09
ORD IDord-ab9a9bde6db94f278edf18209269cd3f
出典メモuspto-grants-1997_09