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Cesium carbonate → Ethyl-7-(4-Benzyl-piperazin-1-yl)-5-fluorobenzofuran-2-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 1-Benzylpiperazine | HCID 75994 | — |
| 反応物 | Binap, (A+-)- | HCID 634876 | — |
| 反応物 | Ethyl 7-bromo-5-fluorobenzofuran-2-carboxylate | HCID 59636759 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Ethyl-7-(4-Benzyl-piperazin-1-yl)-5-fluorobenzofuran-2-carboxylate | HCID 59636706 | — |
反応手順
Benzylpiperazine (1.3 mL, 8.4 mmol), BINAP (0.43 g, 0.69 mmol), Pd2 dba3 (0.32 g, 0.35 mmol), cesium carbonate (3.25 g, 9.76 mmol) were added to a degassed solution of 7-bromo-5-fluoro-benzofuran-2-carboxylic acid ethyl ester (2.0 g, 6.97 mmol) in toluene (50 mL). The mixture was heated at reflux over night. After cooling, the mixture was filtered through a pad of celite and washed with dichloromethane. The filtrate was concentrated under reduced pressure. The product was purified by flash chromatography (SiO2; hexane/EtOAc, 7/3). Yield: 1.6 g (60%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08367676B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-7d7011b0e5ec43758af116dea5115726 |
| 出典メモ | uspto-grants-2013_02 |