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4-Chloro-2-methylphenol → 2-(4-Chloro-2-methyl-phenoxy)-3-methyl-5-nitropyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Chloro-2-methylphenol | HCID 14855 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Chloro-3-methyl-5-nitropyridine | HCID 89648 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(4-Chloro-2-methyl-phenoxy)-3-methyl-5-nitropyridine | HCID 18419461 | — |
反応手順
Sodium hydride (60% in mineral oil, 1.08 g, 27 mmol) was washed 3× with hexanes then a solution of 4-chloro-2-methylphenol (3.50 g, 24.5 mmol) dissolved in tetrahydrofuran (40 mL) was added. The solution was stirred for 20 minutes then 2-chloro-3-methyl-5-nitropyridine (4.02 g, 23.3 mmol) was added and the reaction mixture was heated to reflux for 3 hours. After cooling, the mixture was concentrated in vacuo then dissolved in ethyl acetate and washed with water, 3× with saturated NaHCO3− and saturated NaCl then dried over Na2SO4 and concentrated in vacuo.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06184237B2 |
| 出典データセット | uspto-grants-2001_02 |
| ORD ID | ord-daa795dac1e240708b9450abc8c84188 |
| 出典メモ | uspto-grants-2001_02 |