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Potassium Carbonate → (S)-2-(3-Nitro-benzylamino)-3-phenyl-propionic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Benzene, 1-(bromomethyl)-3-nitro- | HCID 77568 | — |
| 反応物 | Ethyl L-phenylalaninate hydrochloride | HCID 165085 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (S)-2-(3-Nitro-benzylamino)-3-phenyl-propionic acid ethyl ester | HCID 57971682 | 24% |
反応手順
3-Nitrobenzyl bromide (10.0 g, 46 mmol) was dissolved in DMF (180 ml) and potassium carbonate (12.7 g, 92 mmol) added, followed by L-phenylalanine ethyl ester hydrochloride (10.6 g, 46 mmol). The reaction was stirred for 17 h at room temperature before evaporating to dryness. The residue was re-dissolved in EtOAc (150 ml) and washed with water (3×80 ml), dried (Na2SO4) filtered and concentrated to dryness. After purification by flash column chromatography (30% EtOAc/hexane) the product was obtained (3.7 g, 24% yield). LCMS purity 86%, m/z 329 [M++H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07939666B2 |
| 出典データセット | uspto-grants-2011_05 |
| ORD ID | ord-51a06088fd9f44be8bc7c483aca9dec4 |
| 出典メモ | uspto-grants-2011_05 |