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Triethylamine → N-(p-isobutyloxycarbonylaminophenylsulfonyl)methacrylamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methacryloyl chloride | HCID 13528 | — |
| 反応物 | Dimethylacetamide | HCID 31374 | — |
| 反応物 | p-Isobutyloxycarbonylaminophenyl sulfonamide | HCID 18934427 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | N-(p-isobutyloxycarbonylaminophenylsulfonyl)methacrylamide | HCID 18934430 | 58.8% |
反応手順
To a mixture of 54.4 g of p-isobutyloxycarbonylaminophenyl sulfonamide, 40 g of triethylamine, 2 g of N,N-dimethylaminopyridine and 150 ml of N,N-dimethylacetamide was then added dropwise 22.8 g of methacrylic chloride under cooling with ice. After the completion of the dropwise addition, the reaction mixture was stirred for 2 hours. The reaction product was then poured into water. The resulting crystal was then withdrawn by filtration. The crystal was then recrystallized from a 3/7 (by volume) mixture of toluene and ethyl acetate to obtain 40 g of N-(p-isobutyloxycarbonylaminophenylsulfonyl)methacrylamide in the form of white crystal (m.p. 194°-196° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05733707 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-7f1fb53c79494e0b8520d17b81fa2775 |
| 出典メモ | uspto-grants-1998_03 |