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Stannous chloride dihydrate → 4-(4-Cyclohexylphenoxy)-2,5-dimethylaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Stannous chloride dihydrate | HCID 61436 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4-(4-Cyclohexylphenoxy)-2,5-dimethylnitrobenzene | HCID 68596208 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 4-(4-Cyclohexylphenoxy)-2,5-dimethylaniline | HCID 68596076 | 61.5% |
反応手順
A solution of 0.49 g (1.5 mmol) of 4-(4-cyclohexylphenoxy)-2,5-dimethylnitrobenzene in 7 ml of dioxane and 7 ml of hydrochloric acid is admixed with 1.01 g (4.5 mmol) of tin(II) chloride dihydrate at room temperature and the mixture is then refluxed for 2 h. It is cooled to room temperature, neutralized with aqueous NaHCO3 and extracted repeatedly with dichloromethane, and the extracts are dried over Na2SO4 and filtered, and the solvent is removed under reduced pressure. This is followed by purification by column chromatography (0.29 g, purity 95.2%, yield 61.5%, log P (pH 2.3)=4.25).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08748662B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-018238e3bc1740f199fda69cbcf3f27c |
| 出典メモ | uspto-grants-2014_06 |