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14.22 g (100 mmol) of compound II-1 was refluxed in 50 mL of thionyl chloride for 5 hours and then excess thionyl chloride was removed and the resulting residue was dissolved in 20 mL of dry dichloromethane for later use.14.22 g (100 mmol) of compound III-I and 30.36 g (300 mmol) of triethylamine were dissolved in methylene chloride, and the mixture was stirred with cooling in an ice-water bath. Then, a solution ofII-1 acid chloride solution, after the addition was completed, stirring was continued overnight at room temperature.The reaction mixture was poured into 500 mL of ice water, stirred and extracted with 100 mL × 3 dichloromethane. The combined extracts were washed with brine, dried over anhydrous sodium sulfate,The hair was evaporated to dryness and the residue was purified by column chromatography to afford pure product IV-1.
General procedure: Carboxylic acid 3 (0.2 mmol, 1 equiv.) and HATU (0.2 mmol, 1 equiv.) were dissolved in 1 mL DCE in a one dram vial charged with a stir bar. DIPEA (0.1 mL, 0.6 mmol, 3 equiv.) was added and the resulting solution was stirred at RT for 10 minutes. Amine 2 (0.2 mmol, 1 equiv.) was added to the mixture. The reaction solution was heated to 45 °C and stirred overnight. Upon completion the reaction mixture was condensed and loaded onto a 60g C-18 cartridge and purified over a gradient of 5-95percent ACN/H2O. The fractions containing product were identified by LC-MS and condensed under vacuum to give the final product 4. The final product was characterized by NMR.
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