C([O:5][C:6](=[O:38])[CH2:7][CH2:8][CH2:9][S:10]([C:13]1[CH:18]=C(C)[CH:16]=[C:15]([C:20](=[O:37])[N:21]([C:23]2[N:24]=[N:25][C:26]([Cl:36])=[CH:27][C:28]=2[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=2[CH3:35])[CH3:22])[CH:14]=1)(=[O:12])=[O:11])(C)(C)C.C1(OC)C=CC=CC=1.[F:47][C:48]([F:53])([F:52])[C:49](O)=O>ClCCl>[Cl:36][C:26]1[N:25]=[N:24][C:23]([N:21]([CH3:22])[C:20]([C:15]2[CH:14]=[C:13]([S:10]([CH2:9][CH2:8][CH2:7][C:6]([OH:38])=[O:5])(=[O:12])=[O:11])[CH:18]=[C:49]([C:48]([F:53])([F:52])[F:47])[CH:16]=2)=[O:37])=[C:28]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=2[CH3:35])[CH:27]=1To a solution of 4-{3-[(6-chloro-4-o-tolyl-pyridazin-3-yl)-methyl-carbamoyl]-5-methyl-benzenesulfonyl}-butyric acid tert-butyl ester (0.055 g, 89.9 μmol) in dichloromethane (1.5 mL) were added anisole (10.7 mg, 10.8 μL, 98.8 μmol) and trifluoroacetic acid (512 mg, 346 μL, 4.49 mmol) and the light yellow solution was stirred at room temperature for 3.5 hours. The reaction mixture was evaporated to dryness and the residue treated with toluene and again completely evaporated. The product was purified by preparative HPLC (Gemini NX column) using a gradient of methanol:water (containing 0.1% formic acid) (20:80 to 98:2). Colorless foam (0.037 g; 74%). MS (ESI+): m/z=556.09 ([M+H]+).
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