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Methyl iodide → HCID 53986391、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Methyl formate | HCID 7865 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Methyl 2-(4-fluorophenyl)acetate | HCID 2733233 | — |
| 触媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 53986391 | HCID 53986391 | — |
反応手順
Suspend sodium hydride (3.4 g, 142 mmol) in anhydrous tetrahydrofuran (100 mL). Cool in an ice/water bath. Add methyl formate (8.8 mL, 142 mmol), methanol (1 drop), and methyl 4-fluorophenylacetate. Warm slowly to ambient temperature. After 18 hours, concentrate in vacuo to give a residue. Dissolve the residue in dimethylformamide and cool in an ice/water bath. Add methyl iodide (8.0 mL, 130 mmol). Warm slowly to ambient temperature. After 3.5 hours, pour the reaction mixture into water and extract twice with ether. Dry the combined organic layers over MgSO4 filter, and concentrate in vacuo to give the title compound: Rf =0.52 (silica gel, 2/1 hexane/ethyl acetate).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05519048 |
| 出典データセット | uspto-grants-1996_05 |
| ORD ID | ord-a6bd7bc6093740ba97ec9eedac026529 |
| 出典メモ | uspto-grants-1996_05 |