Water → HCID 21852285, compound

Participants

Reaction Conditions

Reaction Steps

Under N2 200 g of 5-chloro-3-nitro-catechol is dissolved in 1050 ml DMF. To this solution are added 204 g anhydrous, powdered K2CO3 and 220 ml CH2Br2, while stirring the mixture. The reaction mixture is refluxed for 1 hour (140° C.) and then cooled down to 80° C. After addition of 800 ml water, the mixture is cooled down to room temp. The crystalline product is filtered off and washed successively with 2×600 ml water, 2×250 ml ethanol, and 2×300 ml n-hexane. After drying under reduced pressure at 60° C., the desired product is obtained in a yield of 82%; purity 95%. Equally successful results are obtained in toluene as the solvent instead of DMF, under phase transfer conditions.

Provenance & Evidence