Iodine → HCID 9962290, compound

Participants

Reaction Steps

Iodine (56 mg, 0.22 mmol) in CH2Cl2 (10 mL) was added over a period of 2 h at 0° C. to 4 (200 mg, 0.20 mmol) in CH2Cl2 (20 mL) under argon. Analysis by TLC (1:2 CH2Cl2 :hexanes) indicated the disappearance of 4. The solution was slowly warmed to room temperature and then washed with NaHSO3 (2×25 mL) and KF solution (1×25 mL), dried (MgSO4), concentrated in vacuo and the residue purified by flash column chromatography (1:6 CH2Cl2 :hexanes) to afford 5 as a pale yellow oil (0.15 g, yield 97%): 1H NMR δ 6.6-7.8 (m, 27 H), 3.78 (s, 2 H), 3.75 (s, 2 H); 13C NMR δ 127-146 (several), 42.24, 40.46; Anal. Calcd for C36H31IS2Sn, C, 55.91; H, 4.04. Found, C, 56.12; H, 4.19.

Provenance & Evidence