Diisopropylethylamine → HCID 58880139, compound

Participants

Reaction Steps

Compound 66 (5.8 g, 12.3 mmol) and DIEA (3.2 mL, 18.4 mmol) were dissolved in toluene (600 mL), and the solution was heated at reflux under N2 for four days. The solution was concentrated and purified by flash chromatography (30% EtOAc/CH2Cl2) to give 4.4 g (87%) of the title compound as a tan solid. 1H NMR (400 MHz, DMSO-d6): δ 12.98 (s, 1H), 8.54 (d, 1H, J=2.4 Hz), 8.20 (d, 1H, J=2.4 Hz), 7.37 (s, 1H), 7.32 (d, 2H, J=8.8 Hz), 6.90 (d, 2H, J=8.8 Hz), 5.25 (s, 2H), 3.71 (s, 3H), 0.39 (s, 9H). MS (ES) [m+H] calc'd for C21H22ClN3O2Si, 412, 414; found 412, 414.

Provenance & Evidence