Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Azobisisobutyronitrile → 3-{[3-(Bromomethyl)-6-chloro-2-fluorophenyl]oxy}-5-chlorobenzonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Azobisisobutyronitrile | HCID 6547 | — |
| 반응물 | N-bromobutanimide | HCID 67184 | — |
| 반응물 | 3-Chloro-5-(6-chloro-2-fluoro-3-methylphenoxy)benzonitrile | HCID 59451640 | — |
| 용매 | Carbon Tetrachloride | HCID 5943 | — |
| 생성물 | 3-{[3-(Bromomethyl)-6-chloro-2-fluorophenyl]oxy}-5-chlorobenzonitrile | HCID 59451576 | 79% |
반응 단계
3-Chloro-5-[(6-chloro-2-fluoro-3-methylphenyl)oxy]benzonitrile (1.8 g, 6.1 mmol) was dissolved in CCl4 (200 mL). NBS (1.2 g, 6.7 mmol) and AIBN (0.63 g, 3.8 mmol) were added and the reaction mixture was placed in oil bath at 85° C. and stirred for 4 h. The reaction was monitored by TLC and more AIBN and NBS were added as necessary. The reaction was cooled, filtered and the solid washed with CCl4. The solvent was evaporated. Purification was accomplished by column chromatography (hexane/EtOAc eluent) to afford the title compound (1.8 g, 79%) as a solid. 1H NMR (400 MHz, DMSO-d6): δ ppm 7.81 (s, 1H), 7.49-7.59 (m, 3H), 7.47 (d, 1H), 4.73 (s, 2H). GC-MS, 372.9 (M).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08304419B2 |
| 출처 데이터셋 | uspto-grants-2012_11 |
| ORD ID | ord-81e8ca9c30bc451ca73ed26f2a9a8f00 |
| 출처 메모 | uspto-grants-2012_11 |