Phosphorus sulfide (P2S5) → HCID 178441312, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of Example 1D (380 mg, 1 mmol) in toluene (25 mL) was added P2S5 (220 mg, 1 mmol) and the reaction mixture was heated at 82° C. for 75 minutes, concentrated under reduced pressure and purified via column chromatography (SiO2, 0-25% EtOAc in hexanes) to provide the title compound (0.14 g, 34% yield). 1H NMR (300 MHz, CDCl3) δ ppm 0.95 (t, J=7.3 Hz, 3 H), 1.40 (dd, J=15.1, 7.5 Hz, 2 H), 1.61-1.78 (m, 11 H), 2.84-3.00 (m, 2 H), 3.84 (s, 3 H), 6.90 (d, J=8.7 Hz, 1 H), 7.27-7.35 (m, 1 H), 7.66 (d, J=2.8 Hz, 1 H), 8.13 (s, 1 H). MS (DCI/NH3) m/z 398 (M+H)+.

Provenance & Evidence