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Dimethyl Sulfate → N-methyl-4-(2-methyl-4-nitrophenoxy)-2-nitrobenzenamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethyl Sulfate | HCID 6497 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Bis(tetrabutylammonium) sulphate | HCID 11433187 | — |
| 反応物 | 4-(2-Methyl-4-nitrophenoxy)-2-nitrobenzenamine | HCID 86650895 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N-methyl-4-(2-methyl-4-nitrophenoxy)-2-nitrobenzenamine | HCID 86650896 | 91% |
反応手順
To a solution of sodium hydroxide (10.2 g in 10.5 mL water) was added toluene (15 mL), 4-(2-methyl-4-nitrophenoxy)-2-nitrobenzenamine (2.00 g, 6.92 mmol), dimethyl sulfate (750 μL, 7.88 mmol) and tetrabutylammonium sulfate (0.277 g, 0.816 mmol). After stirring at room temperature, the cooled (0° C.) reaction mixture was diluted with water (100 mL) and extracted with dichloromethane (100 mL). The organic layer was washed with water and brine, dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was chromatographed (dichloromethane) to provide the product (1.90 g, 91%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08648087B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-84b6540a481e4829af7f3db48c89bdc2 |
| 出典メモ | uspto-grants-2014_02 |