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HRID 446673作成日:2026年10月26日

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

https://huagongshe.com/reaction/446673

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US08481001B2
出典データセットuspto-grants-2013_07
ORD IDord-ee725ae26a1c4ee0ab0d766470fb3701
出典メモuspto-grants-2013_07