関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl Alcohol | HCID 244 | — |
| 反応物 | 4-Methylanisole | HCID 7731 | — |
| 反応物 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Benzyl-1-methoxy-4-methylbenzene | HCID 20549031 | — |
反応手順
A mixture of 4-methylanisole (200 g, 1.64 mol), benzyl alcohol (40.0 g, 0.37 mol) and p-toluenesulfonic acid monohydrate (8.0 g, 0.042 mol) was stirred at 160 to 175° C. for two hours while eliminating water generated by the reaction. After excess 4-methylanisole was distilled off under reduced pressure (inner temperature, 132° C./25 mmHg (3.3 kPa), the residue was dissolved in toluene (50 ml) and then the organic layer was successively washed with water (20 ml), 10% aqueous caustic soda (20 ml) and water (20 ml). After the washed organic layer was concentrated, the residue was distilled under reduced pressure to collect a component fractionated at boiling point of 120-138° C. at 0.7 mmHg (0.09 kPa) as a main fraction (52.75 g, 67.2%). The component was analyzed by NMR to identify 2.7:1 mixture of 2-benzyl-4-methylanisole and 3-benzyl-4-methylanisole.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07268257B1 |
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| 出典データセット | uspto-grants-2007_09 |
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| ORD ID | ord-e1593a35aec94f148dfe91d91a306aad |
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| 出典メモ | uspto-grants-2007_09 |
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