Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Azobisisobutyronitrile → 6-bromomethyl-1-oxo-3-phenyl-1H-indene-2-carboxylic acid ethyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Azobisisobutyronitrile | HCID 6547 | — |
| 반응물 | N-bromobutanimide | HCID 67184 | — |
| 반응물 | 5-Methyl-3-oxo-1-phenylindene-2-carboxylic acid ethyl ester | HCID 68699292 | — |
| 촉매 | Tungsten | HCID 23964 | — |
| 용매 | Carbon Tetrachloride | HCID 5943 | — |
| 생성물 | 6-bromomethyl-1-oxo-3-phenyl-1H-indene-2-carboxylic acid ethyl ester | HCID 68697546 | 36.7% |
반응 단계
6-Methyl-1-oxo-3-phenyl-1H-indene-2-carboxylic acid ethyl ester (3 g, 10.3 mmol) obtained in Step 4 was dissolved in carbon tetrachloride, and N-bromosuccinimide (2 g, 11.4 mmol) and 2,2′-azobisisobutyronitrile (500 mg, 3.09 mmol) were added thereto. The mixture was refluxed for 3 hrs under the irradiation of a 375 W tungsten lamp. Upon the completion of the reaction, the resulting mixture washed with saturated saline and extracted with dichloromethane. The organic layer was separated, dried over anhydrous MgSO4 and concentrated under a reduced pressure. The resulting residue was purified by flash chromatography to obtain 1.4 g of the titled compound (yield: 36.7%) in oil state.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07745439B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-98d8b10c0bda4888ab506e69cf8a6076 |
| 출처 메모 | uspto-grants-2010_06 |