関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Bromhydrol | HCID 166749 | — |
| 反応物 | 2,5-Dimethoxyterephthalonitrile | HCID 12545280 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 2,5-Dihydroxyterephthalonitrile | HCID 643391 | 41.7% |
反応手順
In a 5 liter-reaction vessel, 100 g (5.32×10-1M) of 2,5-dicyano-1,4-dimethoxybenzene, 312.5 g (1.17M) of anhydrous aluminum tribromide and 2.5 liters of dry benzene were placed, followed by heat-refluxing for 7 hours. After the reaction, the reaction mixture as cooled and poured into a mixture of 3 kg of crushed ice and 500 ml of concentrated hydrochloric acid to precipitate a crystal. The crystal was recovered by filtration and dissolved in 2N-sodium hydroxide aqueous solution. The resultant insoluble residue was filtered off and the filtrate was acidified with 2N-hydrochloric acid to precipitate a crystal. The crystal was recovered by filtration and washed with water, followed by drying to obtain 35.5 g of 2,5-dicyanohydroquinone (Yield: 41.7%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05858269 |
|---|
| 出典データセット | uspto-grants-1999_01 |
|---|
| ORD ID | ord-e24c3e1f4a2442379c2b2c8680fe1f38 |
|---|
| 出典メモ | uspto-grants-1999_01 |
|---|