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Dichloromethane → 2-Fluoro-6-octyloxy-3-[4-(4-octyloxyphenyl)phenyl]pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 1-Bromo-4-(4-octoxyphenyl)benzene | HCID 2801787 | — |
| 反応物 | 2-Fluoro-6-octyloxypyridine-3-boronic acid | HCID 19046940 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Fluoro-6-octyloxy-3-[4-(4-octyloxyphenyl)phenyl]pyridine | HCID 19046973 | 13.2% |
反応手順
2.10 g (7.50 mmol) of 2-fluoro-6-octyloxypyridine-3-boronic acid (prepared as described in Example 5) in 35 ml of ethanol are refluxed together with 2.70 g (7.50 mmol) of 4-bromo-4'-octyloxybiphenyl and 0.29 g (0.24 mmol) of tetrakis(triphenylphosphine)palladium in 46 ml of benzene and 2.5 g (23.40 mmol) of sodium carbonate in 11 ml of water for 20 hours. After distributing the reaction mixture between water and dichloromethane, the organic phase is washed with sodium chloride solution, dried over sodium sulfate, filtered and concentrated. Purification of the residue by chromatography (silica gel, dichloromethane) and recrystallization from acetonitrile give 0.50 g of 2-fluoro-6-octyloxy-3-[4-(4-octyloxyphenyl)phenyl]pyridine. ##STR32##
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05630962 |
| 出典データセット | uspto-grants-1997_05 |
| ORD ID | ord-51874d2e1e3549caa257c4049dcb364b |
| 出典メモ | uspto-grants-1997_05 |