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MORPHOLINO(2-NITROPHENYL)METHANONE synthesis

1synthesis methods
110-91-8 Synthesis
Morpholine

110-91-8
678 suppliers
$9.00/1g

61117-58-6 Synthesis
Cobalt, octacarbonyldi-, (Co-Co), stereoisomer

61117-58-6
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Yield:26162-89-0 76%

Reaction Conditions:

with dmap;palladium diacetate;4,5-bis(diphenylphosphino)-9,9-dimethylxanthene in 1,4-dioxane at 90; for 0.333333 h;Sealed tube;Microwave irradiation;

Steps:

General Procedure for the preparation of benzamides.

General procedure: To a dry microwave vial, aryl halide (Br, I) (1 eqv.) and amine (2eqv.) were taken in dry 1,4-dioxane. 5 mol% of Pd(OAc)2, 5 mol% ofXantphos and DMAP (2 eqv.) were added followed by (0.25 or 0.3) equivalents ofCo2(CO)8 and the vial was sealed immediately andmicrowave irradiated for 20 min. The reactionmixture was concentrated under reduced pressure, diluted with ethyl acetate andwater, the ethyl acetate layer separated, dried over sodium sulphate, andconcentrated. Thecrude products obtained were subjected to purification by flash chromatographyon silica gel coloumn eluting with petroleum ether and ethyl acetate.

References:

Baburajan, Poongavanam;Elango, Kuppanagounder P. [Tetrahedron Letters,2014,vol. 55,# 5,p. 1006 - 1010] Location in patent:supporting information

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