ChemicalBook CAS DataBase List 3-NIRO-O-XYLENE

3-NIRO-O-XYLENE synthesis

9synthesis methods

Product Name:3-NIRO-O-XYLENE
CAS Number:616-69-3
Molecular formula:C8H8N2O4
Molecular Weight:196.16

95-47-6 Synthesis

95-47-6
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610-23-1
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616-69-3
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610-03-7
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603-06-5
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Yield:603-06-5 38% ，616-69-3 21% ，610-23-1 17% ，610-03-7 13%

Reaction Conditions:

with Iron(III) nitrate nonahydrate;phosphorus pentoxide in neat (no solvent) at 20; for 6 h;Milling;Green chemistry;

Steps:

General procedure for Table 2 and Table 3

General procedure: A stainless milling beaker of 2.5 mL along with one stainless milling ball ( = 6.0 mm)was used for the reaction. The mechanochemical reaction was performed in a MM400mixer mill at room temperature. A mixture of arene (0.2 mmol), Fe(NO3)3·9H2O (202mg, 0.5 mmol), and P2O5 (213 mg, 1.5 mmol) [For nitrobenzene (Table 2, entry 8), theP2O5 was kept as 284 mg (20 mmol); For methyl benzenesulfonate (Table 2, entry 9),the P2O5 was kept as 426 mg (30 mmol)] were added to the stainless milling beaker,along with one stainless milling ball. The beaker was sealed and placed in the mixermill. The reaction was carried out at 28 Hz for 6 hours. Subsequently, the reactionmixture was dissolved in dichloromethane (15 mL). The resulting mixture was filteredto remove the undissolved residue, and then the solvent was removed via rot-vap undervacuum followed by purification through column chromatography to afford the product.The product was dissolved in a proper deuterium reagent with 7 μl of dibromomethane.The components were analyzed and determined by 1H NMR and literature.

References:

Wu, Jian-Wei;Zhang, Pu;Guo, Zhi-Xin [Tetrahedron Letters,2021,vol. 72,art. no. 153087] Location in patent:supporting information

95-47-6 Synthesis

95-47-6
566 suppliers
$10.00/25g

610-23-1
3 suppliers
inquiry

616-69-3
9 suppliers
inquiry