ChemicalBook CAS DataBase List 2,2'-Oxybis(nitrobenzene)

2,2'-Oxybis(nitrobenzene) synthesis

14synthesis methods

Product Name:2,2'-Oxybis(nitrobenzene)
CAS Number:2217-65-4
Molecular formula:C12H8N2O5
Molecular Weight:260.2

1493-27-2

2217-65-4

General procedure: 1-fluoro-2-nitrobenzene (1.0 mmol) was used as a feedstock, and tributylphosphine (PBu3, 2.0 mmol), palladium acetate (Pd(OAc)2, 2 mol%), and potassium carbonate/zirconium oxide (K2CO3/ZrO2, 1.5 equiv, based on K2CO3, 2.070 g) were added in xylene (10 mL). The mixture was stirred at reflux under nitrogen protection for 24 hours or until TLC showed that the reaction was complete. After completion of the reaction, the mixture was filtered and washed with dichloromethane (DCM). The organic layers were combined and the solvent was removed by evaporation. The product was purified by column chromatography using dichloromethane/hexane (1:1 to 1:2) as eluent to give the target product 2,2'-oxobis(nitrobenzene).

88-73-3 Synthesis

88-73-3
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2217-65-4
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Yield:2217-65-4 98.9%

Reaction Conditions:

with sodium ethanolate in methanol at 45 - 80; for 1.25 h;Large scale;Solvent;Temperature;

Steps:

1-3 Preparation Example 3 of o-nitrophenyl ether:

Add 150 kg of o-nitrochlorobenzene to a 2000L reactor, add 150 kg of methyl alcohol, start stirring to warm up, and when the temperature rises to 48 , start adding the sodium ethoxide solution purchased, according to the concentration of sodium ethoxide purchased (Content 30%) calculate the addition, the addition amount is 1 ~ 1.01 (molar ratio with o-nitrochlorobenzene), the control temperature is not lower than 45 C, not higher than 55 after adding sodium ethoxide solution. Then close all inlets and outlets on the reactor, raise the temperature to 80 °C, the pressure in the reactor is 2.5 ~ 3.5 × 104Pa, and keep it warm for 75 minutes. Then start to distill ethanol at this temperature, while maintaining the temperature, continue to slowly add the recovered washing water, washing the generated sodium chloride, and the amount of washing water added is 300 kg. Then cool down to room temperature. After the product and moisture have dried, the material is dried. The obtained product was 157.3 kg; the melting point of the product was 2.0° C., the product purity: 99.7% (chromatographic analysis); p-nitrophenol: 0.02%; the yield was 98.9%.

References:

CN111187168,2020,A Location in patent:Paragraph 0062-0067

1493-27-2
517 suppliers
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2217-65-4
47 suppliers
$21.00/100mg

References

1493-27-2
517 suppliers
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