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HRID 1992191作成日:2026年10月25日

Sodium Hydroxide → 2,5-Dichloro-3-[(methylsulfonyl)amino]benzoic acid hydrochloride

https://huagongshe.com/reaction/1992191

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium HydroxideHCID 14798—
反応物Chloramben-methylHCID 23714—
反応物Methanesulfonyl chlorideHCID 31297—
反応物DiisopropylethylamineHCID 81531—
反応物Methyl 2,5-dichloro-3-[(methylsulfonyl)amino]benzoateHCID 58727879—
溶媒MethanolHCID 887—
溶媒DichloromethaneHCID 6344—
生成物2,5-Dichloro-3-[(methylsulfonyl)amino]benzoic acid hydrochlorideHCID 68676259—

反応条件

温度0 °C

反応手順

From common intermediate methyl 3-amino-2,5-dichlorobenzoate following the procedure outlined in scheme. Methyl 3-amino-2,5-dichlorobenzoate (2.10 g, 9.55 mmol), DIEA (3.0 ml) were stirred in DCM (40 ml) at 0° C. methanesulfonyl chloride (2.18 g, 19.08 mmol) was added dropwise whike stirring at 0° C. After 2 hrs at 0° C., reaction was allowed to warm to room temperature while stirring overnight. Quenched rxn with saturated NH4Cl and washed with brine. Organic layer with dried to yield crude methyl 2,5-dichloro-3-[(methylsulfonyl)amino]benzoate (3.10 g) which will be carried on. methyl 2,5-dichloro-3-[(methylsulfonyl)amino]benzoate (3.10 g) was treated with NaOH, methanol following procedure outlined in scheme to form 2,5-dichloro-3-[(methylsulfonyl)amino]benzoic acid hydrochloride (3.53 g).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07645771B2
出典データセットuspto-grants-2010_01
ORD IDord-9a67d6355e9c4e71bceeabf93228a865
出典メモuspto-grants-2010_01