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2,4-Dimethylaniline → 2-Bromo-4,6-dimethylaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,4-Dimethylaniline | HCID 7250 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Bromo-4,6-dimethylaniline | HCID 170579 | — |
反応手順
To a solution of 50.0 g (0.413 mol) of 2,4-dimethylaniline in 1500 cm3 of glacial acetic acid, 21.2 ml (65.6 g, 0.410 mol) of bromine was added dropwise with vigorous stirring over ca. 20 minutes. This mixture was stirred for 2 hours at 40° C. The precipitate that formed was filtered off, washed with 50 ml of acetic acid, and dried in air. The resulting white solid was added to a solution of 100 g of potassium hydroxide in 400 ml of water. This mixture was stirred for 30 minutes. The crude product was extracted with 3×100 ml of dichloromethane. The combined extracts were dried over Na2SO4 and evaporated to dryness. Fractional distillation gave yellowish liquid, bp 83-85° C./1 mm Hg. Yield 46.9 g (57%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07868197B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-eaa49f2f895341fca8a82e1070d8be24 |
| 出典メモ | uspto-grants-2011_01 |