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Ammonium Chloride → 2-Benzyl-6-(2-ethoxyethyl)oxypyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 2-Bromo-6-(2-ethoxyethoxy)pyridine | HCID 18182455 | — |
| 反応物 | HCID 178418336 | HCID 178418336 | — |
| 触媒 | Diphenylphosphane;diphenyl(propan-2-yl)phosphane;nickel;chloride | HCID 21654969 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Benzyl-6-(2-ethoxyethyl)oxypyridine | HCID 18182222 | — |
反応手順
A 1.09 mol tetrahydrofuran solution containing benzylmagnesium chloride was slowly added dropwise into a mixture of 1 g of 2-bromo-6-(2-ethoxyethyl)oxypyridine, 145 mg of 1,3-bis(diphenylphosphino)propanenickel(II) chloride and 5 ml of tetrahydrofuran with stirring under ice-cooling in a nitrogen atmosphere. After stirring for 2.5 hours, an aqueous saturated ammonium chloride solution was added thereto and the mixture was extracted with ethyl acetate. The organic phase was further washed with brine, dried over anhydrous sodium sulfate and the solvent was removed. The residue was subjected to silica gel column chromatography using 5% ethyl acetate/hexane as an eluent for separation and purification, to give 1 g of the target compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06599917B1 |
| 出典データセット | uspto-grants-2003_07 |
| ORD ID | ord-cb6d21e19be948e0a7558a6ff7dd6523 |
| 出典メモ | uspto-grants-2003_07 |