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HRID 567724作成日:2026年10月26日

Dimethyl Sulfoxide → 2-(2-Hydroxy-5-nitrobenzyl)-5-methoxy-1-(4-methoxybenzenesulphonyl)-1,2-dihydroindazol-3-one

https://huagongshe.com/reaction/567724

反応式

関与物質

役割名称HCID仕込み量
反応物Dimethyl SulfoxideHCID 679—
反応物WaterHCID 962—
反応物Sodium hydrideHCID 24758—
反応物2-(Chloromethyl)-4-nitrophenolHCID 76305—
反応物5-methoxy-1H-indazol-3-yl 4-methoxybenzenesulphonateHCID 15429047—
生成物2-(2-Hydroxy-5-nitrobenzyl)-5-methoxy-1-(4-methoxybenzenesulphonyl)-1,2-dihydroindazol-3-oneHCID 9805385—

反応手順

5.01 g (15 mmol) of 5-methoxy-1H-indazol-3-yl 4-methoxybenzenesulphonate are dissolved in 70 ml of DMSO and treated in portions with 1.5 g (37.5 mmol) of sodium hydride (60 percent). After stirring for 2 hours, a solution of 2.81 g (15 mmol) of 2-hydroxy-5-nitrobenzyl chloride in 25 ml of DMSO is added dropwise and the mixture is stirred at 90-100° C. for 3 hours. After cooling, 400 ml of water are added, and the mixture is stirred for 3 hours and extracted three times with 400 ml of ethyl acetate. The combined organic phases are washed with 100 ml of water, dried over sodium sulphate, distilled to dryness in vacuo and the residue is recrystallized from ethanol.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06180637B2
出典データセットuspto-grants-2001_01
ORD IDord-c071f75f633949b28c254c8a60b8ebe9
出典メモuspto-grants-2001_01