関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Chlorosulfonic acid | HCID 24638 | — |
| 反応物 | p-tolylmethyl N-(pyrazine-2-carbonylamino)carbamate | HCID 478568 | — |
| 反応物 | 1-(2-Methoxyphenyl)-4-methylpiperazine | HCID 9859120 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-(4-Methylpiperazin-1-yl)-4-methoxybenzene sulfonyl chloride | HCID 54106808 | 71% |
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
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06316450B1 |
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| 出典データセット | uspto-grants-2001_11 |
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| ORD ID | ord-a7c8edddd4ed45baa46af733d2f932a9 |
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| 出典メモ | uspto-grants-2001_11 |
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