関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phenol | HCID 996 | — |
| 反応物 | 4-Hydroxybenzoic acid hydrazide | HCID 1742 | — |
| 反応物 | Benzenamine hydrochloride (1:1) | HCID 8870 | — |
| 反応物 | Phenylparaben | HCID 87250 | — |
| 生成物 | 3,5-Bis(4-hydroxyphenyl)-4-phenyl-1,2,4-triazole | HCID 136026355 | 50% |
反応手順
Into a 500 ml three neck round bottom flask equipped with a magnetic stirbar, nitrogen inlet, glass stopper, and distillation head was placed 4-hydroxybenzoic hydrazide (60.9 g, 0.4 mol) and phenyl-4-hydroxybenzoate (85.7 g, 0.4 mol). The mixture was heated to approximately 220° C. by use of a Wood's metal bath. The solids melt and phenol began to evolve and was removed via the distillation head. After two hours, aniline hydrochloride (103.6 g, 0.8 mol) was added and the temperature was increased to 250° C. and held for two hours. The mixture was cooled and washed repeatedly in methanol to give a white solid (65.8 g, 50% yield). The solid was recrystallized from N,N-dimethylacetamide (approximately 225 ml) to give, after drying at 200° C. under vacuum, white needles (49.7 g, 37% yield) with a melting point of approximately 420° C. by differential thermal analysis (DTA). Elemental analysis for C20H15N3O2 : Calculated: C, 72.93%; H, 4.59%; N, 12.76%; O, 9.72%. Found: C, 72.97%; H, 4.63%; N, 12.84%. This monomer has the following structure: ##STR8##
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05245043 |
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| 出典データセット | uspto-grants-1993_09 |
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| ORD ID | ord-7b40b92986b142c0b4b761dffa4e4a2f |
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| 出典メモ | uspto-grants-1993_09 |
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