Benzene,1-methoxy-2,3-dinitro- synthesis

10synthesis methods

Product Name:Benzene,1-methoxy-2,3-dinitro-
CAS Number:16315-07-4
Molecular formula:C7H6N2O5
Molecular Weight:198.13

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Yield:16315-07-4 100%

Reaction Conditions:

with potassium carbonate at 20; for 14 h;

Steps:

8

A mixture of 2,3-dinitrophenol (5.43 mmol, 1 g), iodomethane (21.7 mmol, 1.35 mL) and K₂CO₃(21.7 mmol, 2.99 g) was stirred at room temperature for 14 h. The reaction was then filtered through celite and the filter bed was washed with additional acetone. The filtrate was concentrated to provide 2,3-dinitroanisole (100%), which was dissolved in a mixture of EtOH/H₂O (1:1, 20 mL) and Fe (19.4 mmol, 1.06 g) and concentrated HCl (8 drops) was added. The mixture was refluxed for 90 min., after which it was filtered through celite and the filter bed was washed with additional EtOH. The filtrate was concentrated and basified (pH>12) with 4 M NaOH and the aqueous layer was extracted with CH₂Cl₂. The organic phase was then separated and washed with brine, dried MgSO₄and concentrated to provide 2,3-diaminoanisole 36b (0.65 g).

References:

US2005/124638,2005,A1 Location in patent:Page/Page column 16