反应详情

To a solution of 4-chlorophenylacetic acid (10.0 g, 58.6 mmol) in CH2Cl2 was added 2-Cert-butyl-1,3-diisopropyl-isourea (50 g, 250 mmol) dropwise at −10° C. The mixture was stirred at room temperature overnight, then the precipitate was, removed by filtration. The filtrate was washed with 1M HCl (aq) and saturated NaCl (aq), dried over Na2SO4, filtered, and concentrated. The residue was purified by silica gel chromatography eluting with 2% EtOAc/petroleum ether to afford the title compound: 1H NMR (CD3OD, 300 MHz) δ 7.26-7.30 (m, 2H), 7.18-7.21 (m, 2H), 3.49 (s, 2H), 1.43 (s, 9H).

1. customremoved by filtration
2. washThe filtrate was washed with 1M HCl (aq) and saturated NaCl (aq)
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified by silica gel chromatography
7. washeluting with 2% EtOAc/petroleum ether