Triethylamine → HCID 178458316, compound

Participants

Reaction Steps

To a solution of Example 82 (70 mg, 0.2 mmol) and triethylamine (120 mg, 1.2 mmol) in dichloromethane cooled in an ice bath was added trifluoroacetic anhydride (125 mg, 0.6 mmol) dropwise. After addition was complete, the mixture was stirred overnight at room temperature. After removal of the solvent, the residue was purified by preparative reverse phase HPLC [Waters 2767; Benetnach 10-C18 20×250 mm, 10 μm; 35-85% acetonitrile/water (0.05% trifluoroacetic acid), 30 mL/minute; detection at 214 and 254 nm] to give the titled compound. 1H NMR (400 MHz, CDCl3) δ ppm 7.33 (t, J=7.85 Hz, 2H), 7.19 (t, J=7.4 Hz, 1H), 7.01 (s, 1H), 6.91 (d, J=7.6 Hz, 2H), 2.01˜2.08 (m, 12H), 1.69 (s, 6H); LCMS (ESI+) m/z 337.7 (M+H)+.

Provenance & Evidence