関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ethyl 4-bromobutyrate | HCID 76300 | — |
| 反応物 | 2-(Trimethylsilyl)ethyl 3-(cyclopropylsulfamoyl)benzoate | HCID 71238446 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(Trimethylsilyl)ethyl 3-[cyclopropyl(4-ethoxy-4-oxobutyl)sulfamoyl]benzoate | HCID 71238737 | 87.7% |
反応手順
A mixture of 2.12 g of 2-(trimethylsilyl)ethyl 3-(cyclopropylsulfamoyl)benzoate, 1.45 g of ethyl 4-bromobutyrate, 2.57 g of potassium carbonate, and 21 mL of DMF was stirred at 80° C. overnight. To the reaction mixture was added water, followed by extraction with ethyl acetate. The organic layer was washed with water and saturated brine in this order, then dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane-ethyl acetate) to obtain 2.48 g of 2-(trimethylsilyl)ethyl 3-[cyclopropyl(4-ethoxy-4-oxobutyl)sulfamoyl]benzoate as a colorless oily substance. ESI+: 456
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09284295B2 |
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| 出典データセット | uspto-grants-2016_03 |
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| ORD ID | ord-bfbae0cf377c43cda65cebf021422f12 |
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| 出典メモ | uspto-grants-2016_03 |
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