Sodium methanethiolate → HCID 59497124, compound

Participants

Reaction Steps

Solid sodium methanethiolate (3.30 g, 47.7 mmol) was added to a 100 mL round-bottomed flask containing a solution of 4-chloro-2-methyl-[1,10]phenanthroline (intermediate obtained previously), (2.10 g, 9.4 mmol) in methanol (50 mL). The reaction mixture was refluxed for 18 hours and allowed to cool down to room temperature afterwards. The solvent was removed in a rotary evaporator and the residue was treated with methylene choride (100 mL) and saturated NaHCO3 (100 mL) and transferred to a separatory funnel. The organic layer was washed with brine (100 mL), dried (Na2SO4), filtered and concentrated in vacuo. The solid residue was treated with ethyl ether, filtered and dried, yielding 1.90 g of a light brown solid (84%).

Provenance & Evidence