Cl.[C:2]([C:6]1[CH:11]=[CH:10][C:9]([NH:12][NH2:13])=[CH:8][CH:7]=1)([CH3:5])([CH3:4])[CH3:3].[C:14](OCC)(=[O:19])[CH2:15][C:16]([CH3:18])=O>C(O)(=O)C>[C:2]([C:6]1[CH:7]=[CH:8][C:9]([N:12]2[C:14]([OH:19])=[CH:15][C:16]([CH3:18])=[N:13]2)=[CH:10][CH:11]=1)([CH3:5])([CH3:3])[CH3:4]4-t-Butylphenylhydrazine hydrochloride (24.2 g, 120 mmol) in acetic acid (600 mL) was stirred with ethyl acetoacetate (16.4 mL, 129 mmol) at 100° C. for 22 hours. The solvent was removed by distillation under reduced pressure, and the resulting solid was recrystallized from chloroform (70 ml, 40° C.)-diethyl ether (200 mL, 0° C.), washed with diethyl ether and dried under reduced pressure to give 21.7 g of the desired product (78% yield).
Wird geladen…