関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Pyrithione | HCID 1570 | — |
| 反応物 | Stearic Acid | HCID 5281 | — |
| 反応物 | Tributylstannane | HCID 5948 | — |
| 反応物 | Phosgene | HCID 6371 | — |
| 反応物 | Azobisisobutyronitrile | HCID 6547 | — |
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 生成物 | Heptadecane | HCID 12398 | 70% |
反応手順
140 mg (1.1 mmol) of N-hydroxypyridine-2-thione in 5 ml of benzene are added dropwise at room temperature under an atmosphere of nitrogen to a solution of 120 mg (1.2 mmol) of phosgene in 5 ml of benzene, and this leads to the instantaneous precipitation of a white solid. 286 mg (1 mmol) of stearic acid and 0.5 ml of pyridine are added in 5 ml of benzene, and the reaction medium is taken to reflux for 4 hours. 3 mmol of tri-n-butylstannane in 5 ml of benzene with 10 mg of AIBN are added to the reaction medium during 10 minutes and refluxing is maintained for 2 and half hours. The reaction is carried out in the presence of tetrachloromethane, iodine and potassium fluoride, as indicated earlier. By filtration on silica (100% pentane), 168 mg of n-heptadecane are obtained. Yield 70%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04668356 |
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| 出典データセット | uspto-grants-1987_05 |
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| ORD ID | ord-a3a33492abd14ad6a02d0bae943facff |
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| 出典メモ | uspto-grants-1987_05 |
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