Water → HCID 21852285, compound

Participants

Reaction Conditions

Reaction Steps

Under N2 8.0 g of NaOH (powdered) is dissolved in 80 ml of DMSO, or, alternatively, in N-methylpyrrolidone (NMP) at 80° C. In about 15 min a solution of 20.0 g of 5-chloro-3-nitro-catechol in 20 ml DMSO (NMP) and 100 ml CH2Cl2 is added at 80° C. The reaction mixture is heated at 130° C. for 8-30 hours while stirring. After cooling down to room temp., successively 200 ml water and 400 ml toluene are added. Stirring for 5 min., separation of the layers, and extraction of the water layer with 100 ml toluene yields a combined organic phase, which is washed twice with 50 ml satd. aqueous NaCl solution, with 50 ml water and twice with 100 ml satd. aqueous NaCl solution. After evaporation of the solvent (100 mbar, 40° C.), the desired product is obtained in a yield of 70.3%; purity 84%.

Provenance & Evidence