関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Butyl phenyl ether | HCID 14311 | — |
| 反応物 | Acid Blue 45 | HCID 72278 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 溶媒 | Boric Acid | HCID 7628 | — |
| 生成物 | 4,8-Diamino-1,5-dihydroxy-3-p-butoxyphenyl-anthraquinone | HCID 20507056 | — |
反応手順
4.0 g of sodium 4,8-diamino-1,5-dihydroxy-anthraquinone-2,6-disulfonate is dissolved in a mixture of 2.0 g of boric acid and 30 ml concentrated sulphuric acid heated to 80° C. The blue solution obtained is cooled to a temperature of 0° to 5° C., and 2.8 g of butoxybenzene is stirred in drop by drop, the colour then changing from blue to reddish brown. The mixture is agitated for a further two hours at 0° to 10° C., then poured onto ice. The suspension obtained is heated on reflux for 4 hours to destroy the boric ester, and a violet precipitate is filtered off after cooling, corresponding to 4,8-diamino-1,5-dihydroxy-3-p-butoxyphenyl-anthraquinone-6-sulphonic acid. The moist precipitate is dissolved hot in a mixture of 24 ml of 33% ammonia and 160 ml of water, and the sulphonic groups are separated by adding 2.2 g of sodium dithionate in stages. The mixture is finally heated to 95° C. for approximately 2 hours, then cooled and filtered. The precipitate thus obtained is washed with slightly acidified water, then with a great excess of water, and dried. The desired product may further be purified by crystallisation or chromatography if necessary.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04376715 |
|---|
| 出典データセット | uspto-grants-1983_03 |
|---|
| ORD ID | ord-7545972047e24fd28517b881a9d21b05 |
|---|
| 出典メモ | uspto-grants-1983_03 |
|---|