참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Lithium Bromide | HCID 82050 | — |
| 반응물 | 2-Bromo-1-(difluoromethoxy)-3-nitrobenzene | HCID 58100766 | — |
| 반응물 | HCID 178418546 | HCID 178418546 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-Difluoromethoxy-6-nitrobenzonitrile | HCID 58100764 | 84.6% |
반응 단계
A mixture of 2-bromo-1-difluoromethoxy-3-nitro-benzene (1 g, 3.7 mmol), CuCN (0.40 g, 4.5 mmol) and LiBr (0.32 g, 3.7 mmol) in tetrahydrofuran (10 ml) are heated in a microwave oven at 200° C. for 40 minutes. The reaction mixture is cooled to ambient temperature, diluted with toluene and washed with aqueous sodium bromide (1M) and aqueous sodium hydrogen sulfite (saturated). The organic phase is dried over sodium sulfate and concentrated. The residue is purified by HPLC to give 2-difluoromethoxy-6-nitrobenzonitrile (0.67 g, 84% yield). 1H-NMR (CDCl3, 400 MHz): 8.20 (d, 1H), 7.85 (t, 1H), 7.75 (d, 1H), 6.75 (t, 1H) ppm.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08524896B2 |
|---|
| 출처 데이터셋 | uspto-grants-2013_09 |
|---|
| ORD ID | ord-47972b48f6ac4d3da12438dc0306f2c1 |
|---|
| 출처 메모 | uspto-grants-2013_09 |
|---|