[F:1][C:2]([F:14])([F:13])[C:3]1[CH:4]=[C:5]([C:9]([NH2:12])([CH3:11])[CH3:10])[CH:6]=[CH:7][CH:8]=1.C(=O)([O-])[O-].[K+].[K+].[Cl:21][CH2:22][C:23](Cl)=[O:24].Cl>ClCCl.O>[Cl:21][CH2:22][C:23]([NH:12][C:9]([CH3:11])([C:5]1[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:13])([F:14])[F:1])[CH:4]=1)[CH3:10])=[O:24]2.5 g (12.3 mmol) of the compound from Example 1A and 1.70 g (12.3 mmol) of potassium carbonate are placed in 30 ml dichloromethane and slowly treated at RT with a solution of 1.46 g (12.9 mmol) of chloroacetyl chloride in 5 ml dichloromethane. The mixture is stirred for 3 hrs at RT and then treated with 150 ml water and slowly with 30 ml 1 N hydrochloric acid. It is extracted three times with dichloromethane. The combined organic phases are dried over magnesium sulphate and freed of solvent on the rotary evaporator. 2.65 g (77% of theory) of the title compound are thus obtained.
Wird geladen…
