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4-Aminophenol → 5,5'-[(1-Methylethylidene)bis(4,1-phenylenoxy)]bis[2-(4-hydroxyphenyl)-1H-isoindole-1,3(2H)-dione]
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Aminophenol | HCID 403 | — |
| 反応物 | 2,2-Bis(4-(3,4-dicarboxyphenoxy)phenyl)propane dianhydride | HCID 94483 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5,5'-[(1-Methylethylidene)bis(4,1-phenylenoxy)]bis[2-(4-hydroxyphenyl)-1H-isoindole-1,3(2H)-dione] | HCID 67238299 | — |
反応手順
247.2 g of 4,4′-(4,4′-isopropylidenediphenoxy)bis(phthalic anhydride) (0.47 mol) are dissolved in 200 ml of DMF in a 3 l three-necked flask with reflux divider, reflux condenser and distillation bridge. 105.8 g of 4-aminophenol (0.095 mol) are slowly added dropwise. The mixture is heated at reflux for 2 hours. Water is continuously removed by distillation during this process. The mixture is then cooled, diluted with 500 ml of dichloromethane, and washed twice with water. Finally, the product is washed with saturated NaCl solution. The organic phase is concentrated, and the residue is brought to the boil in 300 ml of methanol. After cooling, the residue is isolated by suction filtration and then washed with 200 ml of methanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08507635B2 |
| 出典データセット | uspto-grants-2013_08 |
| ORD ID | ord-acdb6b4a0bfe4f0eaa617473d0b03efa |
| 出典メモ | uspto-grants-2013_08 |