関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Acetoxy-2-bromoethane | HCID 13564 | — |
| 反応物 | 3-Fluoro-4-hydroxybenzaldehyde | HCID 587250 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 4-(2-Acetoxyethoxy)-3-fluorobenzaldehyde | HCID 87179406 | 51% |
反応手順
A mixture of 3-fluoro-4-hydroxybenzaldehyde (2.0 g, 14.3 mmol), K2CO3 (5.92 g, 42.8 mmol) and 2-bromoethyl acetate (4.77 g, 28.5 mmol) in acetone (30 mL) is stirred at 55° C. for 24 h before it is diluted with diethyl ether (150 mL) and washed with water (3×50 mL). The organic extract is dried over MgSO4 and concetrated. The remaining residue is chromatographed on silica gel to give the title aldehyde (1.65 g) as a colourless oil. 1H NMR (CDCl3): δ 9.85 (s, 1H), 7.64-7.58 (m, 2H), 7.07 (t, J=8.2 Hz, 1H), 4.49-4.45 (m, 2H), 4.35-4.30 (m, 2H), 2.10 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | USRE045174E1 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-f4d6cc8608e242818de875804781c99a |
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| 出典メモ | uspto-grants-2014_09 |
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