1-Chloro-2,4-Dinitrobenzene → Sodium 2,4-dinitrophenolate

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반응 단계

Sodium 2,4-dinitrophenolate is prepared from 202.6 parts of 2,4-dinitrochlorobenzene in accordance with the statements of Example 1. 92 parts of ammonium chloride are added to the suspension of the 2,4-dinitrophenolate at 70° C., a pH value of 7.1 being established. 290.4 parts of 31.9% strength aqueous hydrosulphide solution are then added in the course of about 20 minutes, whilst stirring and monitoring the pH value. The pH value is reduced from 8.4 to 8.0 by adding a further 92 parts of ammonium chloride, and a further 290.4 parts of 31.9% strength hydrosulphide solution are then added at 70° to 75° C. in the course of about 20 minutes. The pH value thereby rises to 8.4. The reaction mixture is then subsequently stirred at about 70° C. for about 45 minutes. It is cooled to 15° to 20° C., 35 parts of sodium sulphite are added, followed by about 230 parts of 30% strength aqueous hydrochloric acid, in order to adjust the pH to 5. The sulphur-containing 2-amino-4-nitrophenol suspension is subsequently stirred at 5° to 10° C. for about 11/2 hours and is then filtered. 438.4 parts of a 34% strength aqueous paste of 2-amino-4-nitrophenol with a sulphur content of about 19% are obtained. This sulphur-containing filter cake is introduced into a solution of 53 parts of sodium carbonate in 400 parts of water. The mixture is warmed to about 55° to 60° C. and the sulphur is removed from the solution of sodium 2-amino-4-nitrophenolate by filtration. The filtrate is then cooled to about 20° C. and adjusted to pH 5 with about 107 parts of 30% strength aqueous hydrochloric acid. After cooling the mixture to about 5° C., it is filtered. 344 parts of a 42.1% strength aqueous press cake of 2-amino-4-nitrophenol, corresponding to 144.8 parts of 100% pure 2-amino-4-nitrophenol, are obtained. Yield: 94% of theory, relative to 2,4-dinitrochlorobenzene.

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