関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Chloro-6-hydroxyacetophenone | HCID 74061 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-(5-Chloro-2-methoxyphenyl)ethanone | HCID 240434 | 79.1% |
反応手順
Dissolve 5′-chloro-2′-hydroxyacetophenone (15.3594 g, 90.03 mmol) in 100 mL of anhydrous acetonitrile in a pressure vessel. Add K2CO3 (13.7541 g, 99.52 mmol) and MeI (25.56 mL, 180.06 mmol) to the vessel. Seal the vessel and heat the reaction mixture to 85° C. for 18 hours. Cool the reaction and concentrate it in vacuo. Partition the residue between Et2O and H2O. Wash the organic layers with 2N NaOH (2×). Dry the combined organic layers with MgSO4. Filter off the drying agent and concentrate in vacuo to afford 13.15 g of 1-(5-chloro-2-methoxy-phenyl)-ethanone (79%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08552039B2 |
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| 出典データセット | uspto-grants-2013_10 |
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| ORD ID | ord-0f2730e7af154d0b897455ac9f6fb768 |
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| 出典メモ | uspto-grants-2013_10 |
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