反应详情

To a solution of compound (S)-N6, 3-dimethyl-N6-(1-phenylethyl)-[1,2,4]triazolo[4,3-b]pyridazine-6,8-diamine (50 mg, 0.17 mmol) in DCM (10 mL) was added phenyl carbonochloridate (30 mg, 0.19 mmol) dropwise at 0° C. The reaction mixture was stirred at room temperature for 1 h and then the solution of dimethylamine in THF (0.3 mL, 1 N) was added, and the mixture was stirred at room temperature for 2 h. The reaction mixture was diluted with water (15 mL) and extracted with EA (20 mL*3). The combined organic layers were dried over Na2SO4, concentrated in vacuum. The residue was purified by prep-TLC (DCM: MeOH=20:1) to give product (S)-1,1-dimethyl-3-(3-methyl-6-(methyl(1-phenylethyl)amino)-[1,2,4]triazolo[4,3-b]pyridazin-8-yl)urea (Compound 8) as a yellow solid (10 mg, 16.7%). 1H NMR (300 MHz, CDCl3) δ 7.96 (s, 1H), 7.80 (s, 1H), 7.34-7.32 (m, 5H), 3.12 (s, 6H), 2.80 (s, 3H), 2.65 (s, 3H), 1.60 (d, 3H); LRMS (M+H+) m/z: calcd 353.20; found 353.

1. stirringthe mixture was stirred at room temperature for 2 h
2. extractionextracted with EA (20 mL*3)
3. dry with materialThe combined organic layers were dried over Na2SO4
4. concentrationconcentrated in vacuum
5. customThe residue was purified by prep-TLC (DCM: MeOH=20:1)