反应详情

温度

40 °C

To a solution of 1-ethyl-3,3,5-trimethyl-7-{[N-(2-pyridin-3-ylethyl)amino]methyl}-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione (0.5 g), 2-Phenylisobutyric acid (0.24 g), and diisopropylethylamine (0.23 ml) in DMF (10 ml), 2-(7-aza-1H-benzotriazol-1-yl)-1,1,3,3-tetramethyluronium hexafluorophosphate (HATU) (0.50 g) was added and stirred at 40° C. for 10 hours. Water was added to the reaction mixture, and stirred for 1 hour, and, extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue thus obtained was purified by silica gel column chromatography (hexane:ethyl acetate=1:1). The purified product was condensed under reduced pressure. A 1N-hydrogen chloride in ethanol solution was added to a 2-propanol solution (5 ml) of the residue, and the liquid was stirred at room temperature, and concentrated under reduced pressure. Ethanol and ether were added to the residue. The precipitated insoluble matter was separated, washed with ether, and dried to give the title compound (0.35 g) as a white amorphous.

1. stirringstirred for 1 hour
2. extractionextracted with ethyl acetate
3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe residue thus obtained
6. customwas purified by silica gel column chromatography (hexane:ethyl acetate=1:1)
7. customcondensed under reduced pressure
8. stirringthe liquid was stirred at room temperature
9. concentrationconcentrated under reduced pressure
10. additionEthanol and ether were added to the residue
11. customThe precipitated insoluble matter was separated
12. washwashed with ether
13. customdried