Cl.Cl.[NH2:3][C:4]1[CH:12]=[CH:11][C:10]([O:13][CH2:14][CH2:15][CH2:16][N:17]2[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]2)=[CH:9][C:5]=1[C:6]([OH:8])=[O:7].[NH2:23][CH2:24][C:25]([NH:27][CH:28]([CH3:30])[CH3:29])=[O:26].C(N(CC)CC)C.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1>CN(C=O)C.CO>[NH4+:3].[OH-:7].[NH2:3][C:4]1[CH:12]=[CH:11][C:10]([O:13][CH2:14][CH2:15][CH2:16][N:17]2[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]2)=[CH:9][C:5]=1[C:6]([NH:23][CH2:24][C:25](=[O:26])[NH:27][CH:28]([CH3:30])[CH3:29])=[O:8]A mixture of 2-amino-5-(3-piperidin-1-ylpropoxy)benzoic acid dihydrochloride (1.3 g, 3.7 mmol), 2-amino-N-isopropylacetamide*HCl (INTERMEDIATE I.1) (557 mg, 3.7 mmol) and triethylamine (2.1 mL, 14.8 mmol) in DMF (20 mL) was stirred at room temperature for 10 min. EDC (851 mg, 4.4 mmol) and HOBt (600 mg, 4.4 mmol) were added and stirring continued at room temperature for 16 h. The mixture was partitioned between ethyl acetate (100 mL) and 2N Na2CO3 (aq.) (100 mL) and the aqueous extracted with additional ethyl acetate (2×100 mL). The combined organics were washed with brine (1×100 mL), dried (MgSO4), filtered and concentrated in vacuo. The crude residue was purified by chromatography on silica gel with dichloromethane:methanol: NH4OH (aq.) (160:39:1, v/v) as eluent to provide 2-amino-N-(isopropylcarbamoylmethyl)-5-(3-piperidin-1-ylpropoxy)benzamide (INTERMEDIATE V1.1) (1.4 g, 3.7 mmol, 100%).
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