Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Azobisisobutyronitrile → 4-Bromomethyl-1-(2-chloro-phenyl)-5-(4-chloro-phenyl)-1H-pyrazole-3-carboxylic acid ethyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Azobisisobutyronitrile | HCID 6547 | — |
| 반응물 | N-bromobutanimide | HCID 67184 | — |
| 반응물 | Ethyl 1-(2-chlorophenyl)-5-(4-chlorophenyl)-4-methyl-1h-pyrazole-3-carboxylate | HCID 58760952 | — |
| 용매 | Carbon Tetrachloride | HCID 5943 | — |
| 생성물 | 4-Bromomethyl-1-(2-chloro-phenyl)-5-(4-chloro-phenyl)-1H-pyrazole-3-carboxylic acid ethyl ester | HCID 58760946 | 64% |
반응 단계
A mixture of 1-(2-chloro-phenyl)-5-(4-chloro-phenyl)-4-methyl-1H-pyrazole-3-carboxylic acid ethyl ester I-4a (2.8 g, 7.46 mmol), N-bromosuccinimide (1.6 g, 8.95 mmol), AIBN (245 mg, 1.49 mmol) in CCl4 (60 ml) was heated under reflux for 17 hours. The reaction was cooled to room temperature, filtered to remove any solids, and concentrated under vacuum. The crude residue was purified via silica gel chromatorgraphy (Flash 40) using a solvent gradient of 10% EtOAc/hexanes to 20% EtOAc/hexanes to give the desired product (I-4b) as an amorphous solid (2.2 g, 64%): +APCI MS (M+1) 455.0.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07241788B2 |
| 출처 데이터셋 | uspto-grants-2007_07 |
| ORD ID | ord-855fbb13045b45dd9952a942241ecefb |
| 출처 메모 | uspto-grants-2007_07 |