反应详情

To a solution of methyl 3-amino-5-tert-butylpyrrole-2-carboxylate (0.99 g, 5.00 mmol) in anh. CH2Cl2 (50 ml) at room temp. was added a solution of 2,3-dichlorophenyl isocyanate (0.948 g, 5.00 mmol) in CH2Cl2 (10 mL) and the resulting mixture was allowed to stir overnight. The resulting white precipitate formed overnight was separated and washed with CH2Cl2 to give the desired urea (1.39 g, 67%) as a white powder: mp 200-201° C.; 1H-NMR (DMSO-d6) δ1.23 (s, 9H), 3.78 (s, 3H), 6.50 (d, J=2.95 Hz, 1H), 7.26-7.30 (m, 2H), 7.88-7.91 (m, 1H), 9.12 (s, 1H), 9.40 (s, 1H), 10.91 (br s, 1H); FAB-LRMS m/z 384 (M+H). Anal. Calcd for C17H19N3O3Cl2: C, 53.14; H, 4.98; N, 10.94. Found: C, 53.03; H, 4.79; N, 10.86.

1. customThe resulting white precipitate formed overnight
2. customwas separated
3. washwashed with CH2Cl2