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HRID 429135作成日:2026年10月25日

Sodium Carbonate → 3-(4-Methylpiperazin-1-yl)-4-methoxybenzene sulfonyl chloride

https://huagongshe.com/reaction/429135

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Chlorosulfonic acidHCID 24638—
反応物p-tolylmethyl N-(pyrazine-2-carbonylamino)carbamateHCID 478568—
反応物1-(2-Methoxyphenyl)-4-methylpiperazineHCID 9859120—
溶媒DichloromethaneHCID 6344—
生成物3-(4-Methylpiperazin-1-yl)-4-methoxybenzene sulfonyl chlorideHCID 5410680871%

反応条件

温度0 °C

反応手順

2-(4-Methylpiperazin-1-yl)anisole (200 mg, 1 mmol) was added in portions over ten minutes to ice-cooled, stirred chlorosulfonic acid (1.2 ml) under argon. The resulting brown solution was stirred at 0° C. for 0.25 h and then at ambient temperature for a further 1.25 h. The solution was slowly poured onto crushed ice (50 g). Dichloromethane (50 ml) was added to the mixture followed by saturated sodium carbonate solution until pH10 was attained in the aqueous phase. The layers were separated and the aqueous phase further extracted with dicholoromethane. The combined organic phases were dried (Na2SO4) and concentrated to an oil. The oil was stirred with hexane (4 ml) to give the title compound as a cream solid (210 mg, 71%).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06316450B1
出典データセットuspto-grants-2001_11
ORD IDord-a7c8edddd4ed45baa46af733d2f932a9
出典メモuspto-grants-2001_11