関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,6-Dichloro-4-methylphenol | HCID 17077 | — |
| 反応物 | 2-Chloro-N-(4-methylphenyl)acetamide | HCID 27967 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 2-(2',6'-dichloro-4'-methylphenoxy)-N-(4-methylphenyl)acetamide | HCID 57952155 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 溶媒 | Heptane | HCID 8900 | — |
| 生成物 | N-(2',6'-dichloro-4'-methylphenyl)-4-methylaniline | HCID 11369120 | — |
反応手順
12 g (67 mmol) of 2,6-dichloro-4-methylphenol are dissolved in 25 ml of 2-propanol followed by the addition of 10.5 g (76 mmol) of potassium carbonate and 12.8 g (70 mmol) of 2-chloro-N-(4-methylphenyl)acetamide. The mixture is refluxed for 4 h. At this time, the formation of A: 2-(2′,6′-dichloro-4′-methylphenoxy)-N-(4-methylphenyl)acetamide is completed. 13.6 ml of sodium methylate solution 30% in methanol are slowly added and the temperature is increased to about 85° C. by distilling 25 ml of solvent. The mixture is stirred 2 h more to complete the formation of B. 25 ml of water are added at 70° C. to obtain a 2 phases solution. The lower layer is discarded. The upper layer is diluted with 20 ml of heptane-fraction and washed with 2×20 ml of water. The organic phase is separated and concentrated in vacuo to obtain N-(2′,6′-dichloro-4′-methylphenyl)-4-methylaniline as a crude oil. GC/MS: 265 (100, M+), 195 (130).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07906677B2 |
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| 出典データセット | uspto-grants-2011_03 |
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| ORD ID | ord-0161b63b7b774b7187cb7b9c172fc709 |
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| 出典メモ | uspto-grants-2011_03 |
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