関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,5-Dimethyl-p-phenylenediamine | HCID 160824 | — |
| 反応物 | Phenol, 4-(bromomethyl)-2,6-bis(1,1-dimethylethyl)- | HCID 612973 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (4-Amino-2,5-dimethyl-phenylamino)-2,6-di-tert-butyl-phenol | HCID 86759498 | — |
反応手順
4-Bromomethyl-2,6-di-tert-butyl-phenol (2.42 g, 0.008 mole) was dissolved in 50 mL of dry tetrahydrofuran. In a separate conical flask 2,5-dimethyl-benzene-1,4-diamine (2.17 g, 0.016 mole) was dissolved in 25 mL of tetrahydrofuran and solution was transferred to a cylindrical funnel with pressure equalizing tube. Three-necked round-bottom flask containing solution of 4-Bromomethyl-2,6-di-tert-butyl-phenol was kept in oil-bath at 85° C. Solution in the flask was continuously stirred with the help of magnetic stirrer. 2,5-dimethyl-para-phenylene diamine solution was added drop-by-drop, from funnel to the flask in acidic medium for a span of 4-5 hours till all the solution was poured out. The reaction was terminated after that and the final reaction mixture was allowed to attain room temperature. Product was separated by solvent evaporation. The product was purified using silica gel column chromatography. Product was identified by 1H-NMR. The yield of 4-[(4-Amino-2,5-dimethyl-phenylamino)-2,6di-tert-butyl-phenol is 1.86 g (65%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06770785B1 |
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| 出典データセット | uspto-grants-2004_08 |
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| ORD ID | ord-86f04b26e8e04787a808175bb016cfe7 |
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| 出典メモ | uspto-grants-2004_08 |
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