[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([O:8][CH3:9])[C:3]=1[NH:10][C:11](=[O:15])[O:12][CH2:13][CH3:14].C(N(CC)CC)C.Cl[C:24]([O:27]C(Cl)=O)(Cl)Cl>ClCCl>[CH3:9][O:8][C:4]1[C:3]2[N:10]([C:11]([O:12][CH2:13][CH3:14])=[O:15])[C:24](=[O:27])[NH:1][C:2]=2[CH:7]=[CH:6][CH:5]=113.0 g (0.062 mol) ethyl (2-amino-6-methoxy-phenyl)-carbamate and 10.3 mL (0.074 mol) triethylamine in 100 mL dichloromethane are added to a solution of 8.20 mL (0.068 mol) trichloromethylchloroformate in 50 mL dichloromethane while cooling with ice. After 4 hours stirring at ambient temperature the reaction mixture is poured onto ice and extracted with dichloromethane. The combined organic phases are washed with water, dried and freed from the solvent. The residue is stirred in diethyl ether.
Wird geladen…