참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | 4-Chloro-2-toluidine | HCID 7251 | — |
| 반응물 | Potassium Bromide | HCID 253877 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | Sodium;3-oxidodioxaborirane;tetrahydrate | HCID 23693097 | — |
| 촉매 | Ammonium paramolybdate tetrahydrate | HCID 16211167 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-Bromo-4-chloro-6-methylbenzenamine | HCID 20543754 | — |
반응 단계
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)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08026257B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_09 |
|---|
| ORD ID | ord-b3bb722067144d10a04789b67aeacb86 |
|---|
| 출처 메모 | uspto-grants-2011_09 |
|---|
