関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dibenzylamine | HCID 7656 | — |
| 反応物 | Ethyl chloroacetate | HCID 7751 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl 2-(dibenzylamino)acetate | HCID 3553452 | 80% |
反応手順
To a stirred solution of ethyl chloroacetate (1.0 g, 8.16 mmol) in EtOH (5.0 mL), dibenzylamine (2.09 g, 10.6 mmol) was added and the mixture heated at 140° C. in a microwave reactor for 20 min. After evaporation of the solvent, the crude was dissolved in CH2Cl2 and washed with a 1.0 M KOH solution and brine, then dried over Na2SO4, filtered, and concentrated in vacuo to give a crude product, as an oil. Purification by column chromatography using a Teledyne ISCO apparatus, eluting with Cy:EtOAc (98:2), gave the title compound (1.85 g, 80%), as a white solid. MS (ESI) m/z: 284 [M−H]+[1H NMR as previously reported in literature: Synthesis, 1985, 9, 850-855].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09353075B2 |
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| 出典データセット | uspto-grants-2016_05 |
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| ORD ID | ord-86bb5952c5f04e7f9726edcf2814dd69 |
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| 出典メモ | uspto-grants-2016_05 |
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