FIELD: chemistry.
SUBSTANCE: invention relates to a method of producing 2',4,4'-trinitrobenzanilide, which is an intermediate product in the synthesis of 5(6)-amino-2-(4-aminophenyl)benzimidazole - a monomer for producing heat-resistant high-strength fibres. The method includes acylating aniline with 4-nitrobenzoic acid while heating with distillation of reaction water and separating 4-nitrobenzanilide, followed by nitration thereof with nitric acid in a sulphuric acid medium and separating the end product. The method is characterised by that acylation is carried out under pressure at molar ratio of aniline to 4-nitrobenzoic acid of (2-20):1. The 4-nitrobenzanilide is separated in powder form and after nitration thereof, the obtained 2',4,4'-trinitrobenzanilide is separated from the reaction solution by diluting to sulphuric acid concentration of 30-85 wt %. Further, the product is recrystallised from an aromatic solvent or from a mixture of an amide solvent with water.
EFFECT: method cuts the duration of acylation, improves the quality of the product and reduces the amount of wastes.
3 cl, 2 tbl, 8 ex
Title | Year | Author | Number |
---|---|---|---|
METHOD OF OBTAINING 2',4,4'-TRINITROBENZANILIDE FROM 2,4-DINITROANILINE AND 4-NITRO-BENZOYLCHLORIDE | 2013 |
|
RU2547262C2 |
METHOD OF OBTAINING 21,4,41-TRINITROBENZANILIDE | 2006 |
|
RU2348612C2 |
METHOD OF PRODUCING 21,4,41 -TRINITROBENZANILIDE | 2007 |
|
RU2394810C2 |
METHOD OF OBTAINING 5(6)-AMINO-2-(4-AMINOPHENYL)BENXIMIDAZOLE | 2013 |
|
RU2547210C2 |
METHOD FOR PREPARING 5(6)-AMINO-2-(4'-AMINOPHENYL)-BENZIMIDAZOLE | 2005 |
|
RU2283307C1 |
METHOD OF OBTAINING 5(6)-AMINO-2-(4-AMINOPHENYL)BENZIMIDAZOLE FROM 2',4,4'-TRINITROBENZANILIDE | 2013 |
|
RU2547261C2 |
METHOD OF OBTAINING 5(6)-AMINO-2-(4-AMINOPHENYL) BENZIMIDAZOLE | 2006 |
|
RU2345988C2 |
METHOD OF PREPARING P-PHENYLENEDIAMINE | 0 |
|
SU825505A1 |
0 |
|
SU546608A1 | |
METHOD OF PRODUCING CHLORINE-SUBSTITUTED 4,4-DIAMINOBENZANILIDES | 2007 |
|
RU2385861C2 |
Authors
Dates
2015-08-20—Published
2014-06-10—Filed