Dinitolmide synthesis
- Product Name:Dinitolmide
- CAS Number:148-01-6
- Molecular formula:C8H7N3O5
- Molecular Weight:225.16
39614-85-2
148-01-6
The ammoniation process of step C of the present invention is as follows: 400 L of concentrated ammonia (for ammoniation) and 15 kg of ammonium bicarbonate are added to the reactor, and the pre-prepared acyl chloride solution is slowly added to the reactor under stirring. During the reaction, the reaction temperature was controlled below 40℃ by cooling the brine. After the dropwise addition, the reaction was continued with stirring for 1 to 2 hours. Upon completion of the reaction, a filtration operation was carried out, and the filter cake was washed thoroughly with cold water and subsequently dried to obtain 102.6 kg of 3,5-dinitro-o-methylbenzamide, with a yield of 85.9% (in terms of nitro compounds) and a product purity of 98.5%. In step C of the present invention, an ammonia recovery process was designed to reuse ammonia.
39614-85-2
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148-01-6
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Yield:148-01-6 85.9%
Reaction Conditions:
with ammonium hydroxide;ammonium bicarbonate at 40; for 0.5 h;Large scale;
Steps:
6
Step C ammoniated process of the present invention is as follows: in the pot by adding 400L ammoniated concentrated aqueous ammonia and ammonium bicarbonate 15kg, stirring the prepared solution of the acid chloride was added dropwise slowly ammoniated pan, cooled with chilled brine, dropping control to control the reaction temperature below 40 , stirring was continued for 30 minutes after completion of the addition, for 1 to 2 hours, filtration, the product was sufficiently washed with cold water, drying, 3,5-dinitro - o - methyl benzamide 102.6kg, a yield of 85.9% (with respect to the nitro compounds) content of 98.5%.The present invention Buju C, set the ammonia recovery process reuse.
References:
Zhejiang glory Biological Technology Co., Ltd;Chen, Rener;Chen, Jianhua;Zhang, Na;Lu, Hongbo;Huang, Yunqi CN105906523, 2016, A Location in patent:Paragraph 0037; 0041
118-90-1
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148-01-6
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854646-60-9
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148-01-6
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