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ChemicalBook CAS DataBase List 4-(4-Methoxy-3-nitrophenyl)Morpholine
383870-96-0

4-(4-Methoxy-3-nitrophenyl)Morpholine synthesis

4synthesis methods
-

Yield:383870-96-0 95%

Reaction Conditions:

with sulfuric acid;nitric acid in water at 0; for 1 h;

Steps:

1.a

60.0 g Arylmorpholine (0.31 mol) were dissolved in 273 ml 95% sulphuric acid (4.84 mol, 15.6 eq.), while maintaining a temperature between 0-10° C. Stirring at 10° C. was continued for 0.5 h to produce a brown solution which was cooled to ca. -5° C. In a separate flask, 20.9 ml 65% nitric acid (0.34 mol, 0.98 eq.) were added to 30 ml 95% sulphuric acid (0.53 mol, 1.7 eq) precooled to ca. 10° C. This nitrating mixture was then added to the above solution within 1 h ensuring that the temperature remained <0° C. The dark brown reaction mixture was then worked up in a conventional manner (70 g, 95%). The crude product was sufficiently pure to be used directly in the next step.

References:

US2004/138465,2004,A1 Location in patent:Page/Page column 6