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Methyl iodide → (2-Methoxy-1-methoxymethyl-2-ethoxymethyl)-benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-(Phenylmethoxy)-1,3-propanediol | HCID 203567 | — |
| 反応物 | tetrahydrofuran N,N-dimethylformamide | HCID 21974620 | — |
| 生成物 | (2-Methoxy-1-methoxymethyl-2-ethoxymethyl)-benzene | HCID 66890845 | 97% |
反応手順
To a solution of 2-benzyloxy-propane-1,3-diol (5.0 g, 27.4 mmol) in 5:1 THF-DMF (200 mL) at 0° C. was added NaH (1.5 g, 2.3 eq.) followed by methyl iodide (5.1 mL, 3.0 eq.). The resulting white slurry mixture was stirred at room temperature over weekend. The reaction mixture was quenched with sat. NH4Cl, extracted with EtOAc, dried over Na2SO4, filtered, concentrated and the product was purified by chromatography (50% EtOAc/hexanes) to give (2-methoxy-1-methoxymethyl-2-ethoxymethyl)-benzene (5.6 g, 97%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07868002B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-d37a0eca701849719917771c069e3349 |
| 出典メモ | uspto-grants-2011_01 |