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HRID 470527作成日:2026年10月27日

Sodium Carbonate → HCID 42605612、化合物

https://huagongshe.com/reaction/470527

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium CarbonateHCID 10340—
反応物(S)-6-(2-hydroxy-2-methylpropyl)-6-phenyl-3-((S)-1-(4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)ethyl)-1,3-oxazinan-2-oneHCID 59532385—
反応物5-Bromo-1-(cyclopropylmethyl)-1,2-dihydropyridin-2-oneHCID 59635701—
溶媒DimethylformamideHCID 6228—
生成物HCID 42605612HCID 42605612—

反応条件

温度100 °C

反応手順

2 M aqueous Na2CO3 solution (0.84 mL) was added to a solution of (S)-6-(2-hydroxy-2-methylpropyl)-6-phenyl-3-[(S)-1-(4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)ethyl]-1,3-oxazinan-2-one (0.40 g) and 5-bromo-1-cyclopropylmethyl-1H-pyridin-2-one (0.24 g) in dimethyl-formamide (4 mL). The resulting mixture was sparged with argon for 10 min, before [1,1′-bis(diphenylphosphino)ferrocene]-dichloropalladium(II) dichloromethane complex (34 mg) was added. The mixture was heated to 100° C. and stirred at this temperature for 4 h. After cooling to ambient temperature, water was added and the resulting mixture was extracted with ethyl acetate. The combined organic extracts were washed with brine, dried (MgSO4), and concentrated. The residue was purified by chromatography on silica gel (dichloromethane/methanol 99:1->95:5) to afford the title compound that was crystallized with little ethyl acetate. Yield: 0.19 g (46% of theory); Mass spectrum (ESI+): m/z=501 [M+H]+.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08629138B2
出典データセットuspto-grants-2014_01
ORD IDord-076bd0fdac2149e780d465a95cb6dc70
出典メモuspto-grants-2014_01