関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Methylbenzoyl Chloride | HCID 13405 | — |
| 反応物 | 1-Phenylsulfonylpyrrole | HCID 140146 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (1-benzenesulfonyl-1H-pyrrol-2-yl)(4-methylphenyl)ketone | HCID 22928710 | 71% |
反応手順
Under nitrogen atmosphere, to a solution of 1-benzenesulfonyl-1H-pyrrole (284 g, 1.37 mol) in dichloromethane (1.0 L) were added p-toluoyl chloride (318 g, 2.06 mol) and boron trifluoride ether complex (350 g, 2.47 mol), and the mixture was allowed to stand at room temperature for 7 days. The reaction solution was washed successively with 1N aqueous hydrochloric acid solution (750 mL×2), 1N aqueous sodium hydroxide solution (750 mL) and saturated saline (100 mL), dried, and filtered. The filtrate was concentrated under atmospheric pressure until about 500 ml, and thereto was added hexane (500 mL). The reaction mixture was further concentrated until about 500 ml, cooled to 10° C., and the resulting crystals were collected by filtration. The obtained crystals were washed successively with hexane and toluene to give the title compound (315 g, 71%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07425642B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-69e667da46634917ac0f063ee4dba93a |
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| 出典メモ | uspto-grants-2008_09 |
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