関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfate | HCID 6497 | — |
| 反応物 | 1-Aminoanthraquinone | HCID 6710 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 触媒 | Acetic Acid | HCID 176 | — |
| 触媒 | Tetrabutylammonium Bromide | HCID 74236 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Chlorobenzene | HCID 7964 | — |
| 生成物 | Solvent Red 111 | HCID 6706 | 99.5% |
反応手順
A mixture of 1-aminoanthraquinone (purity 99.6%, 22.4 g), monochlorobenzene (224 g), tetra-n-butyl ammonium bromide (3.4 g), 96% potassium hydroxide (11.7 g) and dimethylsulfuric acid (25 g) was stirred while being maintained at 30° C. for 24 hours. After water (150 g) was added, the solution was stirred for 1 hour, being maintained at 50° C. pH of the aqueous phase was 10 or higher. Then, acetic acid (0.5 g) was added for neutralization (pH of the aqueous phase being 7) and then monochlorobenzene was recovered by heating. After being cooled down to 50° C., the solution was filtered, and a solid was washed and then dried to obtain 1-methylaminoanthraquinone (23.7 g, purity 97.6%, yield 97.6%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05017713 |
|---|
| 出典データセット | uspto-grants-1991_05 |
|---|
| ORD ID | ord-b59bfb58a7da4815814fd5d40c8f0650 |
|---|
| 出典メモ | uspto-grants-1991_05 |
|---|