関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phenethylamine | HCID 1001 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Carzenide | HCID 8739 | — |
| 反応物 | Ethyl chloroformate | HCID 10928 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-((2-Phenylethyl)aminocarbonyl)benzenesulfonamide | HCID 19970748 | 67% |
反応手順
20.1 g (0.1 mol) of 4-carboxybenzenesulfonamide were suspended in 300 ml of anhydrous tetrahydrofuran and treated dropwise at 0° C. with stirring with 15.2 ml (0.11 mol) of triethylamine. After 30 min, 10.5 ml (0.11 mol) of ethyl chloroformate were added dropwise at 0° C., the mixture was stirred at this temperature for 1 h, cooled to -10° C. and 12.1 g (0.1 mol, 12.5 ml) of 2-phenylethylamine in 30 ml of anhydrous tetrahydrofuran were added dropwise. After 1 h at 0° C., the mixture was warmed to 20° C. and concentrated in vacuo, the solid residue was treated with water, filtered off with suction and recrystallized from ethanol, and 20.4 g of product were obtained, M.p. 243°-245° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05607954 |
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| 出典データセット | uspto-grants-1997_03 |
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| ORD ID | ord-b4596b61bc464c4a8bfb016e889acaa6 |
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| 出典メモ | uspto-grants-1997_03 |
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