Lawesson's reagent → HCID 57642331, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 2.0 g (0.0053 mole) of 7-bromo-5-(2-chlorophenyl)-1,3-dihydro-8-methoxy-2H-1,4-benzodiazepin-2-one (Id), 200 mL of 1,2-dimethoxyethane and 2.13 g (0.0053 mole) of Lawesson's reagent (2,4-bis(4-methoxyphenyl)-2,4-disulfide-1,3,2,4-dithiadiphosphetane) was heated at 85° C. for 1 hour, then cooled and poured onto ice cold sodium bicarbonate solution. The mixture was extracted twice with ethyl acetate-methanol (9:1), and the organic layers washed successively with water and brine. The combined extracts were dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. Trituration of the residue with ethyl acetate provided 1.7 g of 7-bromo-5-(2-chlorophenyl)-1,3-dihydro-8-methoxy-2H-1,4-benzodiazepin-2-thione (IId). MH+/Z=395.

Provenance & Evidence