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Chloromethyl Methyl Ether → 5-Bromo-3-methoxy-2-(methoxymethoxy)benzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloromethyl Methyl Ether | HCID 7864 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 5-Bromo-2-hydroxy-3-methoxybenzaldehyde | HCID 262238 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-Bromo-3-methoxy-2-(methoxymethoxy)benzaldehyde | HCID 11565322 | 106.8% |
反応手順
Ethyldiisopropylamine (3.01 ml, 17.1 mmol) and methoxymethylchloride (1.5 ml, 15.7 mmol) were added to a dichloromethane solution (30 ml) of 5-bromo-2-hydroxy-3-methoxybenzaldehyde (3.3 g, 14.3 mmol) under ice cooling, and the mixture was stirred at room temperature for 2 hours. The reaction solution was washed with water, dried over magnesium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=3:1→11:9). The purified product was concentrated to dryness under reduced pressure to obtain 5-bromo-3-methoxy-2-methoxymethoxybenzaldehyde (4.2 g) as light yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08598162B2 |
| 出典データセット | uspto-grants-2013_12 |
| ORD ID | ord-d9f9d641b30a4b4b934e7049a3b737e3 |
| 出典メモ | uspto-grants-2013_12 |