* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
General procedure: The title compounds were prepared in a parallel fashion by thefollowing protocol: Step 1: To a 0.325M solution of amino acid in DMF (400 muL, 125 mumol, 1 eq) was added a 0.325M solution of 4-tert-butyl-1,2-diaminobenzene in DMF (400 muL, 125 mumol, 1 eq), a 0.325M solutionof HATU in DMF (400 muL, 125 mumol, 1 eq) and triethylamine(35 muL, 250 5 mumol, 2 eq). The reaction was shaken at 60 °C for 16 hbefore concentrating in vacuo. To the residue was added HOAc(1.25 mL) and the reaction shaken at 80 °C for 3 h. The reaction wascooled, concentrated in vacuo and purified using preparative HPLC toafford the benzimidazole intermediate. Step 2: To the benzimidazolewas added a solution of TFA/DCM (1:5, 2 mL) and the reaction wasshaken at 30 °C for 1 h. The reaction was concentrated in vacuo to affordthe final compounds as their TFA salts. LCMS QC: Column: Welch XBC182.1x50mm 5 pm, 50 °C, mobile phase A: 0.0375percent TFA in water;mobile phase B: 0.01875percent TFA in acetonitrile. Initial gradient 15 1percent B;0.60 mins 5percent B, 4.00 mins 100percent B, 4.30 mins 1percent B, 4.70 mins 1percent B.Flow rate 0.8 mL/min. Preparative HPLC: Phenomenex Gemini C18;250x21.2mmx10um; Acetonitrile:NH4OH eluting with a gradient specificto each compound (see below) over an 8?10 min gradient time.Flow rate 30/35 mL/min unless otherwise specified.
Chemistry
Pharmaceutical Intermediates
Inhibitors/Agonists
Material Science
For Research Only
120K+ Compounds
Competitive Price
1-2 Day Shipping
