Sodium Carbonate → HCID 67900548, compound

Participants

Reaction Steps

75 parts of 3-hydroxyethylsulfonyl-2-nitrobenzoic acid are added at a steady rate over a period of 30 minutes with stirring to a mixture of 40 parts of iron powder and 200 parts of water heated to 80° to 85° C., and the reaction temperature of the mixture is maintained at 80° to 85° C. during the addition. After the addition is completed, the mixture is stirred for 30 minutes, brought to a pH of 8.5 with aqueous sodium carbonate solution and is clarified while hot by filtering off precipitated iron hydroxide. The filter residue is washed twice with a small amount of hot water. The combined filtrates are then acidified with 25 parts of glacial acetic acid, concentrated in vacuo to 150 parts by volume and subsequently cooled to 0° to 5° C. with stirring. The slightly brownish precipitate is isolated on a nutsche filter, washed with a small amount of icewater and dried at 60° C. in vacuo. This gives 78 parts of 3-hydroxyethylsulfonylanthranilic acid acetate of the formula ##STR15## of melting point 286° to 289° C. and a purity by diazotization) of 99.5%.

Provenance & Evidence