反应详情

To a solution of 3,5-Diiodobenzohydrazide (4.5 g, 11.60 mmol) in dry THF/DMF (100.0 ml:24.0 ml) was slowly added 3-methoxybenzoyl chloride (2.2 g, 12.90 mmol) at 0° C. under nitrogen. After addition of 3-methoxybenzoyl chloride, the reaction was warmed up to room temperature. The reaction mixture was stirred for 19 hours at room temperature and then pyridine (5.0 ml) was added and stirred for additional 1 h. Water (300.0 ml) was added to reaction mixture. The white solid was obtained and collected by filtration. After dried under vacuum, product was obtained as white powder in 5.05 g (83.3%). 1H NMR (400 MHz, DMSO-d6, δ): 10.72 (s, 1H, NH), 10.62 (s, br, 1H, NH), 8.33 (t, J=1.6 Hz, 1H), 8.23 (d, J=1.6 Hz, 2H), 7.50-7.41 (m, 3H), 7.15 (m, 1H), 3.81 (s, 3H, OCH3).

1. customat 0° C.
2. stirringstirred for additional 1 h
3. customThe white solid was obtained
4. filtrationcollected by filtration
5. customAfter dried under vacuum
6. customproduct was obtained as white powder in 5.05 g (83.3%)