참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 2-Bromophenol | HCID 7244 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Dimethyl 2-fluoroterephthalate | HCID 79178 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Dimethyl 2-(2-bromophenoxy)benzene-1,4-dicarboxylate | HCID 57839250 | — |
반응 단계
A mixture of 2-fluoro-terephthalic acid dimethyl ester 2j (10 g, 47.1 mmol), 2-bromophenol 1j (6.0 mL, 51.8 mmol) and potassium carbonate (7.16 g, 51.8 mmol) in N,N-dimethylformamide (100 mL) was heated at 100° C. for 36 h. The mixture was allowed to cool to rt, then poured into cold dilute hydrochloric acid (0.5 N, 350 mL). The product was extracted into EtOAc, washed with water (4×) and brine (1×) and dried over magnesium sulfate. The solvent was evaporated in vacuo, and the residue was purified by flash chromatography on silica gel using dichloromethane as the eluant. The crude product was isolated (10.5 g) and used without further purification in the subsequent reaction. MS: m/z 365 (MH+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08106207B2 |
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| 출처 데이터셋 | uspto-grants-2012_01 |
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| ORD ID | ord-9aa268fa9af64837b4fe9febf42eaf06 |
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| 출처 메모 | uspto-grants-2012_01 |
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