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Ammonium Chloride → 1-(2-Methoxyphenyl)-3-methyl-1-(3-methyl-2-pyridyl)-2-buten-1-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 1-Bromo-2-methyl-1-propene | HCID 98560 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 反応物 | 2-(2-Methoxybenzoyl)-3-methylpyridine | HCID 19895690 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-(2-Methoxyphenyl)-3-methyl-1-(3-methyl-2-pyridyl)-2-buten-1-ol | HCID 19895660 | 59.4% |
反応手順
9.23 g of 1-bromo-2-methylprop-1-ene were added dropwise to 2.5 g of magnesium turnings covered with tetrahydrofuran while heating. 7.76 g of 2-methoxyphenyl 3-methyl-2-pyridyl ketone were added while heating to reflux. After 4 hours the mixture was allowed to cool to room temperature. Saturated ammonium chloride solution was added and the resulting mixture was extracted with diethyl ether. The organic extract was dried over sodium sulphate and evaporated. The residue was chromatographed on silica gel using ethyl acetate/petroleum ether (1:4) for the elution. There were obtained 5.75 g of 1-(2-methoxyphenyl)-3-methyl-1-(3-methyl-2-pyridyl)-2-buten-1-ol in the form of an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05118694 |
| 出典データセット | uspto-grants-1992_06 |
| ORD ID | ord-a2126e63cfbe4f268809752ef17f8c01 |
| 出典メモ | uspto-grants-1992_06 |