反应详情

温度

140 °C

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].

1. customAfter evaporation of the solvent
2. dissolutionthe crude was dissolved in CH2Cl2
3. washwashed with a 1.0 M KOH solution and brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customto give a crude product
8. customPurification by column chromatography
9. washeluting with Cy