[Cl:1][C:2]1[N:7]=[N:6][C:5]([NH:8][CH3:9])=[C:4]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[CH3:16])[CH:3]=1.[C:17]([O:21][C:22]([CH2:24][CH2:25][CH2:26][S:27]([C:30]1[CH:31]=[C:32]([CH:36]=[C:37]([C:39](F)(F)F)[CH:38]=1)[C:33](O)=[O:34])(=[O:29])=[O:28])=[O:23])([CH3:20])([CH3:19])[CH3:18]>CCCCCCC.C(OCC)(=O)C>[C:17]([O:21][C:22](=[O:23])[CH2:24][CH2:25][CH2:26][S:27]([C:30]1[CH:38]=[C:37]([CH3:39])[CH:36]=[C:32]([C:33](=[O:34])[N:8]([C:5]2[N:6]=[N:7][C:2]([Cl:1])=[CH:3][C:4]=2[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[CH3:16])[CH3:9])[CH:31]=1)(=[O:29])=[O:28])([CH3:18])([CH3:19])[CH3:20]The title compound was prepared in analogy to example 1, from (6-chloro-4-o-tolyl-pyridazin-3-yl)-methyl-amine (example 4, intermediate a) and 3-(3-tert-butoxycarbonyl-propane-1-sulfonyl)-5-trifluoromethyl-benzoic acid after a reaction time of 18 hours and using a gradient of n-heptane:ethyl acetate (100:0 to 30:70) for the chromatographic purification. Another purification step using preparative HPLC (Gemini NX column) with a gradient of methanol:water with 0.05% formic acid (80:20 to 98:2) yielded the desired compound as a colorless solid (14%). MS (ESI+): m/z=541.090 ([M+H]+).
Wird geladen…