Trichloroacetyl isocyanate → HCID 24821336, compound

Participants

Reaction Steps

To a solution of Example 1F (0.15 g, 0.0004 mol) in methylene chloride (5 mL) was added trichloroacetyl isocyanate (0.08 mL, 0.0006 mol) and the mixture was stirred at room temperature for 15 minutes, and concentrated. The residue was dissolved in methanol (10 mL) and refluxed with a few drops of saturated sodium carbonate solution for 0.5 hours. The mixture was cooled to room temperature, concentrated to dryness and triturated with methanol (15 mL) and water (2 mL) to give 0.15 g of the title compound (88% yield). 1H NMR (300 MHz, DMSO-d6) δ ppm 1.23-1.34 (m, 9 H) 4.55-4.75 (m, 2 H) 5.42 (s, 2 H) 6.44 (d, J=8.09 Hz, 1 H) 6.97-7.05 (m, 2 H) 7.25-7.36 (m, 4 H) 7.49 (d, J=8.09 Hz, 2 H) 7.65 (s, 1 H). MS (ESI), m/z 397.9 (M+H)+.

Provenance & Evidence