Sodium sulfide nonahydrate → HCID 22629952, compound

Participants

Reaction Steps

1-bromo-4-methyl-2-nitrobenzene (3 mmol) dissolved in DMF (3 mL) was combined with a solution of sodium sulfide nonahydrate (3 mmol) in water 3 (mL) and stirred for 48 hours. A solution of 5-chloro-6-(chloromethyl)-1,3-benzodioxole (3 mmol) in ethyl acetate (5 mL) was added in and the reaction was agitated for another 24 hours. The reaction was diluted with ethyl acetate and washed sequentially with 0.5 N NaOH solution (7 mL×1), water (7 mL×3) and brine (7 mL×1). The solvent was removed under a stream of nitrogen and the residue crystallized from a mix of dichloromethane and hexane.

Provenance & Evidence