Water → HCID 21484312, compound

Participants

Reaction Steps

A solution of triethylammonium 4-hydroxydithiocarbanilate (28.6 g) in dimethylformamide (100 ml) is added to a mixture of methylene bromide (52.2 g), triethylamine (10.1 g) and dimethylformamide (200 ml) over a 15-minute period while the temperature is being kept below 30° C. The mixture is stirred overnight, poured into water and the aqueous mixture extracted with benzene. The benzene solution is washed, dried, and stripped to yield 12.5 g (63.5% of theory) crude product, as a brown solid. The crude product is dissolved in hot methanol (100 ml) and the solution allowed to stand in the cold one day to yield 4.9 g of a bone-white solid, melting point 162° C to 163° C.

Provenance & Evidence