関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Propionyl chloride | HCID 62324 | — |
| 反応物 | 2,3-Dimethylanisole | HCID 76269 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Carbon Disulfide | HCID 6348 | — |
| 生成物 | 1-Propanone, 1-(4-methoxy-2,3-dimethylphenyl)- | HCID 13306696 | 91.7% |
反応手順
To a stirred solution of 2,3-dimethylanisole (197.0 g) and propionyl chloride (147.0 g) in carbon disulfide (700 ml) is added anhydrous aluminum chloride (232.0 g) at 5°-10° C. over a period of 1.5 hours. Stirring is continued for 2 hours under cooling and additional 3 hours at room temperature. The reaction mixture is poured onto crushed ice--concentrated hydrochloric acid with stirring. The mixture is extracted with chloroform and the chloroform solution is washed successively with water, dilute sodium bicarbonate solution and water and then dried over anhydrous sodium sulfate. After removal of the solvent by evaporation, the residue is distilled at 121°-126° C. (1-2 mmHg) to give the title compound (255.0 g), which is crystallized from n-hexane, m.p. 39°-40° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04528299 |
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| 出典データセット | uspto-grants-1985_07 |
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| ORD ID | ord-e821cf1d067e446f94e7cc973f1392ee |
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| 出典メモ | uspto-grants-1985_07 |
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