関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Aminophenol | HCID 403 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Fluoro-4'-(phenylethynyl)benzophenone | HCID 4095657 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | 4-(4-Aminophenoxy)-4'-phenylethynylbenzophenone | HCID 23352813 | 85% |
反応手順
In a 250 mL flask equipped with nitrogen inlet, overhead stirring assembly, Dean-Stark trap, and reflux condenser were placed 4-aminophenol (5.46 g, 0.05 mol), 4-phenylethynyl-4'-fluorobenzophenone (15.02 g, 0.05 mol), potassium carbonate (7.6 g, 0.055 mol), toluene (20 mL), and DMAc (45 mL). The mixture was heated to 150° C. for 2 h, then cooled to room temperature. The reaction mixture was poured into water and the resulting light yellow powder was collected by filtration. Recrystallization from toluene afforded the desired product in 85% yield: m.p. 151°-153° C. IR (KBr); 3382 and 3314 cm-1 (NH2); 3049, 1599, and 1509 cm-1 (aromatic C--H); 2217 cm-1 (C=C); and 1645 cm-1 (C=O): Mass Spec. m/e (relative intensity): M+, 389.4 (100); FW=389.44 g/mol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05412066 |
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| 出典データセット | uspto-grants-1995_05 |
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| ORD ID | ord-c9bf34767f6240c1b6e5fc3d71b4a948 |
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| 出典メモ | uspto-grants-1995_05 |
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