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Chemical Structure| 69938-56-3 Chemical Structure| 69938-56-3

Structure of 69938-56-3

Chemical Structure| 69938-56-3

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Product Details of [ 69938-56-3 ]

CAS No. :69938-56-3
Formula : C7H7NO4
M.W : 169.14
SMILES Code : NC1=CC(C(O)=O)=C(O)C=C1O
MDL No. :MFCD10699567
InChI Key :WCDMNZRFRZYKDG-UHFFFAOYSA-N
Pubchem ID :18380150

Safety of [ 69938-56-3 ]

GHS Pictogram:
Signal Word:Warning
Hazard Statements:H302-H312-H332
Precautionary Statements:P261-P264-P270-P271-P280-P301+P312-P302+P352-P304+P340-P330-P363-P501

Application In Synthesis of [ 69938-56-3 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 69938-56-3 ]

[ 69938-56-3 ] Synthesis Path-Downstream   1~2

  • 1
  • [ 13722-96-8 ]
  • [ 69938-56-3 ]
YieldReaction ConditionsOperation in experiment
63% In a 250 mL four-necked flask equipped with a thermometer and a spherical condenser, 4 g of 5-nitro-2,4-dihydroxybenzoic acid, 0.28 g of Pd / C catalyst, and 60 mL of ethanol were added in a dropwise manner using a constant pressure dropping funnel. 7mL of hydrazine hydrate, heated to reflux temperature, reacted for 4h, stopped heating, filtered the reaction solution while it was hot, and filtered the filtrate into an ice-water bath to cool down for 30min. Add 0.1g of stannous chloride, then add 100mL of concentrated hydrochloric acid, and let stand for 6h , Filtered, and the filter cake was dried to obtain an off-white product. The mass fraction by HPLC analysis was 94.83%, and the yield based on 5-nitro-2,4-dihydroxybenzoic acid was 66.12%.
61.22% With sodium dithionite; water; sodium hydroxide; at 10 - 30℃; for 2h;Large scale; 1000 g of 5-nitro 2,4-dihydroxybenzoic acid was dissolved in 10 L of 5%In aqueous sodium hydroxide solution, add to a 20L four-necked flask and stir to cool to 10-15 C.Start adding 3500 g of sodium dithionite in batches at a temperature of 20-30 C.The system gradually precipitated a yellow solid.When sodium dithionite is added to one third, the system precipitates yellow-green solids which are relatively viscous and difficult to stir.Continue to add about one-third of sodium dithionite, the system is no longer sticky,After the addition was completed, the reaction was stirred at 20-30 C for 2 h (central control 1).The above steps are the key to successful nitro reduction. The inventor of the present application found thatThe effect of adding sodium dithionite to the reaction system in one time is not ideal, and it needs to be added in batches.The amount of each addition should not exceed half of the total amount.It is best not to exceed one third of the total amount (added more than three times), and,The temperature is preferably controlled at 20-30 C.Such a reaction system does not cause a low yield due to viscous or the like.After the reaction is completed, it is filtered, blasted at 60 C for 5 h, and 20 L at 20-30 C for 2 h.After filtration, it was air-dried at 60 C (central control 2).The crude product was beaten with 8 L of water at 20-30 C, filtered and blast dried at 60 C.Obtained 520g of gray solid, (central control 3)The HPLC purity was 98.78%, and the yield was 61.22%.
  • 2
  • [ 108-46-3 ]
  • [ 69938-56-3 ]
 

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