Lawesson's reagent → HCID 87209109, compound

Participants

Reaction Steps

To a stirred solution of Example 21 (0.06 g, 0.15 mmol) in THF (10 mL) at r.t. was added 2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane 2,4-disulphide (0.06 g, 0.15 mmol). The reaction mixture was stirred for 2 h and then poured into aqueous sat. NaHCO3 solution (50 mL) and extracted with DCM (2×50 mL). The combined organic fractions were dried over MgSO4, filtered and the solvent removed in vacuo to give the title compound (0.02 g, 35%) as an orange solid. δH (DMSO-d6) 10.33 (1H, br. s), 7.63 (1H, d, J 8.0 Hz), 7.10 (2H, m), 6.86 (1H, d, J 8.0 Hz), 4.16 (1H, br. s), 3.98 (1H, d, J 8.0 Hz), 3.73 (2H, m), 3.57 (3H, m), 3.31 (1H, m), 3.01 (1H, m), 2.74 (2H, s), 2.57 (2H, d, J 5.6 Hz), 2.40 (3H, s), 1.04 (6H, s). LCMS (ES+) 426.9 (M+H)+.

Provenance & Evidence