関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-Methylcyclohexylamine | HCID 7514 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 4-Chlorobutyryl chloride | HCID 78370 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-Chloro-N-cyclohexyl-N-methylbutanamide | HCID 13208297 | — |
反応手順
To ethyl acetate (400 ml) is added N-methylcyclohexylamine (26 ml), and to the mixture are added dropwise with stirring 4-chlorobutyryl chloride (25 ml) and triethylamine (33.5 ml) over a period of 20 minutes with keeping the inner temperature at 10° to 20° C. by ice-cooling. The mixture is further stirred at room temperature for one hour. After the reaction, water is added to the reaction mixture. The organic layer is separated and washed with water an aqueious saturated potassium carbonate solution, 10% aqueous hydrochloric acid and water in order, and then dried over anhydrous sodium sulfate. After filtering off sodium sulfate, the mother liquor is concentrated and distilled under reduced pressure to give N-methyl-N-cyclohexyl-4-chlorobutyramide (41.5 g), b.p. 133°-136° C./2 mmHg.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04766120 |
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| 出典データセット | uspto-grants-1988_08 |
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| ORD ID | ord-d3926ad918984844bf5b7332cf93bba8 |
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| 出典メモ | uspto-grants-1988_08 |
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