Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Azobisisobutyronitrile → 1-bromo-6-methoxy-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 | 6-methoxy-3-phenyl-1H-indene-2-carboxylic acid ethyl ester | HCID 11845112 | — |
| 촉매 | Tungsten | HCID 23964 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1-bromo-6-methoxy-3-phenyl-1H-indene-2-carboxylic acid ethyl ester | HCID 68698470 | 74% |
반응 단계
6-Methoxy-3-phenyl-1H-indene-2-carboxylic acid ethyl ester (1.5 g, 5.10 mmol) prepared in Preparation Example 1 was dissolved in dichloromethane (80 mL), and N-bromosuccinimide (1.09 g, 6.12 mmol) and 2,2′-azobisisobutyronitrile (0.08 mg, 0.51 mmol) were added thereto. The mixture was stirred for 2 hrs at RT under the irradiation of a 375 W tungsten lamp. Upon the completion of the reaction, the 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 (ethyl acetate/n-hexane=1/20→1/9) to obtain 1.4 g of the titled compound (yield: 74%) as a yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07745439B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-dbb54efd464f4ac8818e337f503f8cdb |
| 출처 메모 | uspto-grants-2010_06 |