関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | p-Fluorophenethylamine | HCID 4653 | — |
| 反応物 | 4-(Chlorosulphonyl)benzoyl chloride | HCID 82024 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-[2-(4-Fluoro-phenyl)-ethylcarbamoyl]-benzenesulfonyl chloride | HCID 86609820 | — |
反応手順
TEA (474 μL, 3.4 mmol), is added dropwise to a suspension of the title A compound, 4-chlorosulfonyl-benzoyl chloride in DCM (10 mL) at −78° C. To this mixture is added p-fluorophenethylamine over 5 min. After another 10 min at −78° C., the solution is allowed to warm to 0° C. and stirring is continued at this temperature for 1 h. The reaction is quenched by adding it to ice-water (30 mL), and the mixture is extracted with DCM (3×10 mL). The combined organic phases are dried over anhydrous magnesium sulfate, filtered, and concentrated under vacuum to obtain the crude product which is chromatographed on silica gel using EtOAc as the eluent to give 4-[2-(4-fluoro-phenyl)-ethylcarbamoyl]-benzenesulfonyl chloride.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07700637B2 |
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| 出典データセット | uspto-grants-2010_04 |
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| ORD ID | ord-dd90f2032a8d4d06b81842de02cda08b |
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| 出典メモ | uspto-grants-2010_04 |
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