反应详情

Combine 3-amino-1H-1,5-benzodiazepine-2,4-(3H, 5H)-dione (5.60 g, 29.3 mmol), 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimde hydrochloride (6.75 g, 35.2 mmol) and 4(dimethylamino)pyridine (0.183 g, 1.5 mmol) in 100 mL DMF, add 4,4,4-trifluoro butyric acid dropwise at 0-5° C. After addition, stir the reaction mixture at ice-water. After half an hour, warm to RT. After stirring overnight, remove solvent DMF under reduce pressure and suspend the residue in 200 mL of mixed solvent (CHCl3: i-PrOH=3:1). Collect the solid via vacuum filtration to give the title compound (6.87 g, yield 74%): mass spectrum (APCI) (m/e): 316.1 (M+1); 1H NMR (400 MHz, DMSO-d6): δ 10.72 (s, 2H), 8.60 (d, 1H, J=7.2 Hz), 7.24-7.15 (m, 4H), 4.74 (d, 1H, J=7.2 Hz), 2.58 (t, 2H, J=7.2 Hz), 2.39-2.35 (m, 2H).

1. additionAfter addition
2. waitAfter half an hour
3. customremove solvent DMF
4. customCollect the solid
5. filtrationvia vacuum filtration