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Ethyl Acetate → Methyl 2-(2-chloro-4-methylphenoxy)-2-phenylacetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 2-Chloro-4-methylphenol | HCID 14851 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Methyl 2-(2-bromophenyl)acetate | HCID 8063364 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 2-(2-chloro-4-methylphenoxy)-2-phenylacetate | HCID 19385673 | 83.1% |
反応手順
To a suspension of 0.282 g (7.04 mmol) of a 60% oil dispersion of sodium hydride in DMF was added 1.00 g (7.04 mmol) of 2-chloro-4-methylphenol and the mixture was stirred under an N2 atmosphere at room temperature. After 10 minutes, a solution of 1.94 g (8.45 mmol) of methyl 2-bromophenylacetate dissolved in 10 mL of DMF was added and the reaction was stirred an additional 1.5 hours. The reaction was then diluted into ethyl acetate, washed with water, dried (MgSO4), filtered and evaporated. The residue was purified on a silica gel flash chromatography column eluted with 4% ethyl acetate/hexane to afford 1.70 g (83%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05401745 |
| 出典データセット | uspto-grants-1995_03 |
| ORD ID | ord-cd49721ed4c64165be330ebe474c3f22 |
| 出典メモ | uspto-grants-1995_03 |