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Vanillin → 3-Methoxy-4-(methoxymethoxy)benzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Vanillin | HCID 1183 | — |
| 反応物 | Chloromethyl Methyl Ether | HCID 7864 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 溶媒 | Acetophenone | HCID 7410 | — |
| 生成物 | 3-Methoxy-4-(methoxymethoxy)benzaldehyde | HCID 79661 | 53.1% |
反応手順
To 14.0 g of vaniline and 51.0 g of potassium carbonate was added 280 ml of acetophenone, and chloromethyl methyl ether was further added and the mixture was refluxed for 1 hour. The reaction liquid was cooled to room temperature and filtered, and the filtrate was concentrated under reduced pressure. The reaction mixture was dissolved in ether, washed with water, shaken with a saturated aqueous solution of sodium chloride, dried with anhydrous sodium sulfate and concentrated under reduced pressure. The concentrate was subjected to the column chromatography [230-400 mesh Kieselgel; eluting solvent=hexane/ethyl acetate (2/1)] to obtain 9.6 g (yield=53.1%) of 3-methoxy-4-methoxymethoxybenzaldehyde.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05106871 |
| 出典データセット | uspto-grants-1992_04 |
| ORD ID | ord-eb2a940fb7c54570abe6147f97a86483 |
| 出典メモ | uspto-grants-1992_04 |