反应详情

2,5-Dichloro-4-methyl-nitrobenzene (50 g, 0.24 mol) was heated at reflux, in tetrahydrofuran (200 ml), with t-butoxy-bis(dimethylamino)methane (63.3 g, 0.364 mol) for 8 hours. The reaction mixture was cooled to room temperature and slowly poured into hexanes (3L) with stirring. The desired product was collected by filtration as a dark red solid, 36.9 g, 58% yield. mp 173°-5° C. NMR (CDCl3) δ 8.01 (s, 1), 7.32 (s, 1), 7.08 (d, 1), 5.27 (d, 1), 3.00 (s, 6). Analysis Calculated for C10H10N2O2Cl2 : C, 45.99; H, 3.86; N, 10.73, Found: C, 45.91; H, 3.72; N, 10.61.

1. filtrationThe desired product was collected by filtration as a dark red solid, 36.9 g, 58% yield