関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzene hexane | HCID 110624 | — |
| 反応物 | 2-(Chloromethyl)-1-methyl-4-nitrobenzene | HCID 187952 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Methyl-5-nitrobenzyl acetate | HCID 12940761 | — |
反応手順
A slurry of anhydrous sodium acetate (60.0 g; 0.73 mol) in acetic acid (400 ml) is stirred and 2-methyl-5-nitrobenzyl chloride (45.3 g; 0.24 mol) added. The resulting reaction mixture is heated to reflux and is heated overnight at 115° C., after which time tlc (silica gel; 75/25 hexane/benzene) indicates that no starting material is present. The mixture is cooled down, concentrated in vacuo, and diluted with water. The precipitated solid (48.9 g; 95.8%) is collected and dried. A sample recrystallized from hexane has a melting point of 52°-53.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04430114 |
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| 出典データセット | uspto-grants-1984_02 |
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| ORD ID | ord-25feafc9070146f49ae4c1ce2acbaf1c |
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| 出典メモ | uspto-grants-1984_02 |
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