[CH2:1]([O:8][C:9](=[O:21])[NH:10][C:11]1([C:14](=O)/[N:15]=[CH:16]/[N:17](C)C)[CH2:13][CH2:12]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.Cl.[NH2:24]N.CCOC(C)=O.O>CC(O)=O>[CH2:1]([O:8][C:9](=[O:21])[NH:10][C:11]1([C:14]2[NH:15][CH:16]=[N:17][N:24]=2)[CH2:13][CH2:12]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1To a solution of (1-{[1-dimethylamino-meth-(E)-ylidene]-carbamoyl}-cyclopropyl)-carbamic acid benzyl ester (1.11 g, 3.83 mmol) in AcOH (6 ml) was added hydrazine dihydrochloride (803 mg, 7.65 mmol). The reaction mixture was stirred at 90° C. for 1.5 h. The reaction mixture was poured into EtOAc/water. The organic phase was separated, washed with water, sat. NaHCO3, brine, dried over anhydrous Na2SO4, filtered, concentrated and dried under high vacuum to afford 677 mg of [1-(4H-[1,2,4]triazol-3-yl)-cyclopropyl]-carbamic acid benzyl ester as a off-white solid, m/z 259.6 [M+1]+.
Wird geladen…
