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Chemical Structure| 33513-44-9 Chemical Structure| 33513-44-9

Structure of 33513-44-9

Chemical Structure| 33513-44-9

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Product Details of [ 33513-44-9 ]

CAS No. :33513-44-9
Formula : C7H4Na2O7S2
M.W : 310.21
SMILES Code : O=S(C1=CC=C(C=O)C(S(=O)([O-])=O)=C1)([O-])=O.[Na+].[Na+]
MDL No. :MFCD00043913
Boiling Point : No data available
InChI Key :UUKHCUPMVISNFW-UHFFFAOYSA-L
Pubchem ID :169512

Safety of [ 33513-44-9 ]

GHS Pictogram:
Signal Word:Warning
Hazard Statements:H315-H319
Precautionary Statements:P264-P280-P302+P352+P332+P313+P362+P364-P305+P351+P338+P337+P313

Application In Synthesis of [ 33513-44-9 ]

* 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 [ 33513-44-9 ]

[ 33513-44-9 ] Synthesis Path-Downstream   1~3

  • 1
  • [ 57497-39-9 ]
  • [ 33513-44-9 ]
  • disodium 4-((tert-butylimino)methyl)benzene-1,3-disulfonate N-oxide [ No CAS ]
YieldReaction ConditionsOperation in experiment
86% With sodium methylate; In methanol; water; isopropyl alcohol; EXAMPLE 3 Preparation of alpha-(2,4-disulfophenyl)-N-tert-butylnitrone Disodium Salt Using an 100percent Isopropanol Premix, Condensation Reaction, Ethyl Acetate Distillation, Water Adjustment, Filtration and Drying Process. Sodium methoxide (156.8 g, 2.90 equiv.) in isopropanol (0.5 L) was added to <strong>[57497-39-9]N-tert-butylhydroxylamine hydrochloride</strong> (379.2 g, 3.0 equiv.) in isopropanol (2.45 L), then stirred for 20 minutes. The mixture was filtered and the solid then washed with isopropanol (0.5 L). The filtrate and washings were added to a suspension of 4-formyl-1,3-benzenedisulfonic acid disodium salt (814.5 g) in methanol (7.36 L) and water (0.49 L) in a 12 L jacketed reactor fitted with reflux condenser and overhead stirrer. After 7.5 hours reflux, an additional amount of sodium methoxide (15.6 g) in isopropanol (245 mL) was added to <strong>[57497-39-9]N-tert-butylhydroxylamine hydrochloride</strong> (37.9 g) in isopropanol (50 mL), mixed and filtered and the filtrate added to the reaction reflux and reflux continued a further 4 hours. The reaction was cooled and sodium methoxide (12.0 g) was added and the reaction mixture then stirred for 20 minutes. The solution was then transferred using a peristaltic pump through an in-line filter into a 12 L jacketed vessel, fitted for distillation with a stillhead adapter, condenser and an overhead stirrer. The mixture was distilled at such a rate to maintain an approximately constant volume while isopropanol:water (99:1) was added. A total of 10 L of distillate was collected and 10 L of isopropanol:water (99:1) was added. The suspension was cooled to ambient temperature. Water (400 mL) was added and the mixture was stirred, then filtered. The white solid was washed with isopropanol (2*200 mL) then dried in a fluid bed dryer at 100° C. for about one hour to give the required product (86percent yield). HPLC (percent area): 98.3percent alpha-(2,4-disulfophenyl)-N-tert-butylnitrone disodium salt; 0.30percent 4-formyl-1,3-benzenedisulfonic acid disodium salt; 0.70percent 4-formyl-1,3-benzenedisulfonic acid disodium salt dimethyl acetal; chloride (ISE, w/w): 0.68percent.
  • 2
  • [ 57497-39-9 ]
  • [ 33513-44-9 ]
  • 2,4-disulfonyl-α-phenyl-N-tertiary-butylnitrone disodium salt [ No CAS ]
  • 3
  • [ 15307-93-4 ]
  • [ 33513-44-9 ]
  • C31H19Cl4N2O6S2(1-)*Na(1+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
0.93 g Exemplified Compound 11 (0091) <strong>[15307-93-4]2,6-dichlorodiphenylamine</strong> (4.86 g) and 4-formylbenzene-1,3-disodium disulfonate (3.17 g) were heated at a temperature of 60° C. for 50 hours in the presence of sulfuric acid (10.00 g) in water (20 mL) for reaction to give a reaction liquid. The obtained reaction liquid was cooled to room temperature, the reaction liquid was discharged onto ice (100 g), and then chloroform was added for liquid separation to extract the aqueous phase. To the obtained aqueous phase, manganese oxide (2.90 g) was added, and then the mixture was stirred at a temperature of 20 to 25° C. for 24 hours for reaction to give a reaction liquid. To the filtrate obtained by filtering the obtained reaction liquid, 2 mol/L of sodium hydroxide aqueous solution was added to adjust the pH of the liquid to 7.0. Thereafter, sodium chloride was added for salting-out, and then the precipitated solid was fractionated by filtration. The obtained solid was added into methanol (100 mL), the filtrate obtained by filtration was concentrated under reduced pressure, and then the resultant mixture was purified by column chromatography to thereby give Exemplified Compound 11 (0.93 g) represented by the following structural formula. Exemplified Compound 11 (0092) (0093) It was confirmed that the obtained Exemplified Compound 11 had the above-described structure by [2] LC/TOFMS analysis. The analysis results are shown below. [2] LC/TOF MS Analysis (Eluate: 0.1percent Acetic Acid Aqueous Solution-Methanol, ESI) Results: (0094) Retention time 14.2 minutes: Purity=98.1percent by area, m/z=718.9463 (M-Na)?
 

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