1,2-Dichloroethane → HCID 178429201, compound

Participants

Reaction Steps

The product from Example 39, Step 2 (210 mg, 1.129 mmol, 1.0 equiv) was combined with the product from Example 4, Step 2 (300 mg, 1.129 mmol, 1.0 equiv), EDC (260 mg, 1.355 mmol, 1.2 equiv) and Et3N (189 μL, 1.355 mmol, 1.2 equiv) in DMF (3 mL) and stirred at room temperature for 18 hours. The reaction mixture was diluted with EtOAc and 1N HCl. The phases were separated, and the organic phase was washed twice with 1N HCl, once with satd. NaHCO3, and once with satd. NaCl. The organic phase was concentrated en vacuo. The residue was purified by flash chromatography (20-100% EtOAc in Hexanes) and further purified by reverse-phase HPLC (17-90% CH3CN/H2O, 0.1% TFA over 13 minutes, retention time 7.5 min) to provide 125 mg (26%) of the title compound as a white solid. MS (ES+) m/e 434 [M+H]+

Provenance & Evidence