反应详情

To a solution of 1-ethyl-3,3,5-trimethyl-7-[(2-pyridine 3-ylethylamino)methyl]-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione(0.5 g), 1-methyl-3-indoleacetic acid(0.27 g), and 1-hydroxybenzotriazole (HOBT) (0.24 g) in acetonitrile (10 ml), N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (WSC) (0.30 g) was added and stirred at room temperature for 3 days. The reaction mixture was concentrated under reduced pressure. Ethyl acetate and water were added to the residue 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=1:3→0:1). The purified product was condensed under reduced pressure. A 1N-hydrogen chloride in ethanol solution (1.1 ml) 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(0.26 g) as a pale orange white amorphous.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additionEthyl acetate and water were added to the residue
3. extractionextracted with ethyl acetate
4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue thus obtained
7. customwas purified by silica gel column chromatography (hexane:ethyl acetate=1:3→0:1)
8. customcondensed under reduced pressure
9. stirringthe liquid was stirred at room temperature
10. concentrationconcentrated under reduced pressure
11. additionEthanol and ether were added to the residue
12. customThe precipitated insoluble matter was separated
13. washwashed with ether
14. customdried