[NH2:1][C:2]1[N:6]([CH3:7])[N:5]=[C:4]([C:8]([O:10][CH3:11])=[O:9])[CH:3]=1.ClC(Cl)(O[C:16](=[O:22])OC(Cl)(Cl)Cl)Cl.CCN(C(C)C)C(C)C.[CH2:33]([NH2:37])[CH:34]([CH3:36])[CH3:35]>C1COCC1>[CH2:33]([NH:37][C:16](=[O:22])[NH:1][C:2]1[N:6]([CH3:7])[N:5]=[C:4]([C:8]([O:10][CH3:11])=[O:9])[CH:3]=1)[CH:34]([CH3:36])[CH3:35]To a solution of methyl 5-amino-1-methyl-1H-pyrazole-3-carboxylate (compound 351.4, 0.088 g, 0.57 mmol) in THF (5 ml) was added triphosgene (0.084 g, 0.28 mmol) followed by DIEA (0.2 ml, 1.14 mmol). After the mixture was stirred at room temperature for 2 hours, isobutyl amine (0.225 ml, 2.28 mmol) was added. The resulting mixture was stirred at room temperature over night. The mixture was partitioned between water and EtOAc. The EtOAc layer was washed with 1 M aqueous NaH2PO4 solution followed by brine, dried with Na2SO4, and concentrated to give 120 mg (83%) of a light yellow solid. m/z (ES+) 255 (M+H)+.
読み込み中…
