関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Acrylamide, N-cyclohexyl- | HCID 137811 | — |
| 反応物 | Thiourea | HCID 2723790 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | N-Cyclohexyl-3-sulfanylpropanamide | HCID 14618019 | 90.4% |
反応手順
A mixture of N-cyclohexylacrylamide (15.3 g), concentrated hydrochloric acid (19.4 g, 37.6%), thiourea (7.6 g) and water (10 g) was heated to 60° C. for 2 hours, cooled to 20° C. and sodium hydroxide (50%, 16 g) was slowly added under nitrogen keeping the temperature below 30° C. The resulting mixture was heated to 60° C. for 1 hour and extracted with methylene chloride (2×50 ml). Removal of the solvent afforded N-cyclohexyl-3-mercaptopropionamide (16.9 g) which was purified by vacuum distillation at 0.05 mm and 130° C. to yield 13.7 g of N-cyclohexyl-3-mercaptopropionamide; m.p. 73.5°-75.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04868310 |
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| 出典データセット | uspto-grants-1989_09 |
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| ORD ID | ord-53ae26dce11243889025a43cfbcb42ac |
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| 出典メモ | uspto-grants-1989_09 |
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