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HRID 336801作成日:2026年10月25日

Acetic Acid → N-(3-{[2-chloro-6-(methyloxy)pyridin-4-yl]amino}quinoxalin-2-yl)-3-nitrobenzenesulfonamide

https://huagongshe.com/reaction/336801

反応式

関与物質

役割名称HCID仕込み量
反応物Acetic AcidHCID 176—
反応物Dimethyl SulfoxideHCID 679—
反応物Sodium MethoxideHCID 10942334—
反応物N-{3-[(2,6-dichloropyridin-4-yl)amino]quinoxalin-2-yl}-3-nitrobenzenesulfonamideHCID 57448672—
溶媒WaterHCID 962—
溶媒Ethyl AcetateHCID 8857—
生成物N-(3-{[2-chloro-6-(methyloxy)pyridin-4-yl]amino}quinoxalin-2-yl)-3-nitrobenzenesulfonamideHCID 57448664—

反応条件

温度100 °C

反応手順

To a crude product of N-{3-[(2,6-dichloropyridin-4-yl)amino]quinoxalin-2-yl}-3-nitrobenzenesulfonamide (1.24 g) prepared using procedures similar to those for Example 151, was added anhydrous DMSO (10 mL), followed by sodium methoxide (273 mg). The resulting mixture was heated at 100° C. for 3 days. The mixture was diluted with EtOAc and water, and the pH was adjusted to about 4 by adding acetic acid. The product was extracted with EtOAc (3×). The combined extracts were washed with brine to give the crude product. A portion of the crude product was purified by prep HPLC to give N-(3-{[2-chloro-6-(methyloxy)pyridin-4-yl]amino}quinoxalin-2-yl)-3-nitrobenzenesulfonamide. 1H NMR (400 MHz, DMSO) δ 9.44 (s, 1H), 8.90 (s, 1H), 8.50 (d, 1H), 8.42 (d, 1H), 7.88-7.84 (m, 2H), 7.77 (s, 1H), 7.74 (s, 1H), 7.64 (d, 1H), 7.45-7.38 (m, 2H), 3.82 (s, 3H); MS (EI) m/z for C20H15ClN6O5S: 496.94 (MH+).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08889664B2
出典データセットuspto-grants-2014_11
ORD IDord-0d21021e536941e5b5037f602f3446df
出典メモuspto-grants-2014_11