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Benzyl Bromide → Methyl 4-benzyloxy-3-nitrobenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzyl Bromide | HCID 7498 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Benzoic acid, 4-hydroxy-3-nitro-, methyl ester | HCID 66835 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | Methyl 4-benzyloxy-3-nitrobenzoate | HCID 289857 | — |
反応手順
A solution of 4-hydroxy-3-nitro-benzoic acid methyl ester (30 g, 152 mmol) in acetone (1000 mL) was charged into a 2 L reactor and treated with K2CO3 (31.5 g, 228 mol) and benzyl bromide (52 g, 36.1 mL, 304 mmol). The mixture was mechanically stirred at heated at reflux for 16 hours under a light argon flux. After cooling to room temperature the solvent was evaporated. The residue was taken up in ethyl acetate/water and the two phases were separated. The aqueous phase was extracted three times with ethyl acetate (total solvent volume: 1.5 L, total water volume 1 L). The combined organic phases were dried over sodium sulfate and evaporated. 4-Benzyloxy-3-nitro-benzoic acid methyl ester thus obtained was used crude in the following reaction.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08030308B2 |
| 出典データセット | uspto-grants-2011_10 |
| ORD ID | ord-7cddeaed8130442db8fbd55c3661e0c9 |
| 出典メモ | uspto-grants-2011_10 |