Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,2-Dibromobenzene → 2'-Bromobiphenyl-3-carboxylic acid ethyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,2-Dibromobenzene | HCID 11414 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | (3-Ethoxycarbonylphenyl)boronic acid | HCID 3249312 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 용매 | 2-Methylphenethyl alcohol | HCID 88267 | — |
| 생성물 | 2'-Bromobiphenyl-3-carboxylic acid ethyl ester | HCID 58730981 | 67.8% |
반응 단계
A mixture of 1,2-dibromobenzene (0.63 ml, 5.2 mmol), (3-ethoxycarbonylphenyl)boronic acid (506 mg, 2.6 mmol), tetrakis(triphenylphosphine)palladium(0) (640 mg, 0.6 mmol) and potassium carbonate (2.879 g, 20.9 mmol) was heated in toluene-ethanol (1:1, 10 ml at 90° C. for 3 hours. Upon cooling, the mixture was diluted with ethyl acetate and water. The layers were separated and the aqueous phase was extracted with ethyl acetate. The combined extracts were dried (Na2SO4), filtered and concentrated. The residue was purified by chromatography using Biotage with iso-hexane containing a gradient of DCM (2-15%) to yield the title compound (538 mg, 34%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07446222B2 |
| 출처 데이터셋 | uspto-grants-2008_11 |
| ORD ID | ord-f00d8cdedfc244c2b1157fa02a493e53 |
| 출처 메모 | uspto-grants-2008_11 |