関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-Bromophenol | HCID 7244 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Dimethyl 2-fluoroterephthalate | HCID 79178 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Dimethyl 2-(2-bromophenoxy)benzene-1,4-dicarboxylate | HCID 57839250 | — |
反応手順
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+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08106207B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-9aa268fa9af64837b4fe9febf42eaf06 |
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| 出典メモ | uspto-grants-2012_01 |
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