反应详情

To a mixture of 2,4-dinitrobenzaldehyde (6.45 g, 32.9 mol) and K2CO3 (5.45 g, 39.4 mmol) in DMIF (60 mL) was slowly added methyl thioglycolate (3.0 mL, 32.9 mmol). The mixture was stirred at RT for 1 h, then at 50° C. for 2 h. The resultant mixture was poured into H2O/ice and stirred until a precipitate formed. The solid was filtered and triturated with hot MeOH. The pale brown solid was filtered. 1H NMR (DMSO-d6) δ 9.13 (s, 1H), 8.33 (s, 1H), 8.30-8.17 (m, 2H), 3.89 (s, 3H). MS (EI): cal'd (MH+) 238.01, exp (MH+) 238.10.

1. waitat 50° C. for 2 h
2. stirringstirred until a precipitate
3. customformed
4. filtrationThe solid was filtered
5. customtriturated with hot MeOH
6. filtrationThe pale brown solid was filtered