関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 4-Chloro-2-toluidine | HCID 7251 | — |
| 反応物 | Potassium Bromide | HCID 253877 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Sodium;3-oxidodioxaborirane;tetrahydrate | HCID 23693097 | — |
| 触媒 | Ammonium paramolybdate tetrahydrate | HCID 16211167 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Bromo-4-chloro-6-methylbenzenamine | HCID 20543754 | — |
反応手順
4-Chloro-2-methylaniline (1.0 g, 7.06 mmol), potassium bromide (1.01 g, 8.47 mmol), and ammonium heptamolybdate tetrahydrate (87 mg, 0.07 mmol) were suspended in acetic acid (7 mL, 122 mmol) and cooled to 0° C. The reaction was treated with sodium perborate tetrahydrate (1.2 g, 7.77 mmol), stirred at 0° C. for 30 min, and at room temperature for 2 h. The mixture was poured into water, neutralized with saturated sodium bicarbonate and extracted with ethyl acetate (2×). The organic layers were pooled together, washed with brine (2×), dried over sodium sulfate, and concentrated to afford 1.2 g (78%). 1H-NMR (CDCl3, 500 MHz) δ 7.28 (s, 1H), 6.97 (s, 1H), 4.03 (bs, 2H), 2.17 (s, 3) Mass spec.: 221.90 (MH)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08026257B2 |
|---|
| 出典データセット | uspto-grants-2011_09 |
|---|
| ORD ID | ord-b3bb722067144d10a04789b67aeacb86 |
|---|
| 出典メモ | uspto-grants-2011_09 |
|---|
