関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 2,4-Dimethylphenol | HCID 7771 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,3-Dichloro-1,4-dimethyl-5-nitrobenzene | HCID 13772927 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 3-Chloro-2-(2,4-dimethylphenoxy)-1,4-dimethyl-5-nitrobenzene | HCID 14820605 | 69.6% |
反応手順
Into a round bottom reaction flask equipped with a magnetic stirrer, condenser, thermometer and nitrogen inlet was added 50.0 grams (0.23 mol) of 2,5-dimethyl-3,4-dichloronitrobenzene, 38.5 grams (0.32 mol) of 2,4-dimethylphenol, 50 grams (0.36 mol) of potassium carbonate and 125 milliliters of dimethylformamide. The reaction mixture was heated to a temperature of 90° C.-100° C. and maintained at this temperature for a period of 72 hours. The reaction mixture was then cooled, filtered and concentrated to give a dark oil. The dark oil was partitioned between toluene (300 milliliters) and 4% sodium hydroxide (250 milliliters) and then separated. The organic layer was washed with water and brine, dried over Na2SO4 and concentrated to give a dark oil. The dark oil was trituated with hexane and a solid was formed. The solid was washed with cold hexane and vacuum dried to give 47.8 grams (0.16 mol) of 4-(2,4-dimethylphenoxy) 2,5-dimethyl-3-chloronitrobenzene as a tan powder having a melting point of 78° C.-80° C. Elemental analysis of the tan powder indicated the following:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05420163 |
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| 出典データセット | uspto-grants-1995_05 |
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| ORD ID | ord-403b3b6d780f4d52ba8ef616caf6a946 |
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| 出典メモ | uspto-grants-1995_05 |
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