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Oxygen → 2-Iodo-4-methylaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Oxygen | HCID 977 | — |
| 反応物 | p-Toluidine | HCID 7813 | — |
| 反応物 | Ammonium dihydrogen phosphate | HCID 24402 | — |
| 反応物 | Ammonium iodide | HCID 25487 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Iodo-4-methylaniline | HCID 2764000 | 82% |
反応手順
To a 500-ml pressure-proof glass autoclave were added 150 g (1.03 mole) of ammonium iodide, 5 g (0.0262 mole) of copper iodide, 50 g (0.435 mole) of ammonium dihydrogenphosphate, 70 g (0.654 mole) of p-toluidine, 250 ml of benzene and 100 ml of pure water, and reaction was carried out with stirring under a condition that the oxygen pressure be 3 to 8 kg/cm2 (gauge pressure) and the temperature be 70° C. At the point when the oxygen pressure decreased from 8 kg/cm2 to 3 kg/cm2, oxygen was supplied again to 8 kg/cm2. After 3 hours, the organic layer was taken out, and 83.1 g (0.357 mole) of 2-iodo-4-methylaniline was obtained from this layer. The yield was 82%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04487752 |
| 出典データセット | uspto-grants-1984_12 |
| ORD ID | ord-961b19d042b04344a862309947376ab6 |
| 出典メモ | uspto-grants-1984_12 |