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Typical applications of Bredereck's reagent(3) |
2022-06-19 |
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To a solution of ketones 13b-d (1.3 mmol) in anhydrous DMF (2.5 mL),
TBDMAM (0.41 mL, 2 mmol) was added and the reaction mixture was irradiated under microwave conditions(Power 50 W; Pressure 100 psi; Temperature 100 C) up to completeness (TLC).
In both cases, the reaction mixtures was poured onto crushedice.
The precipitate was filtered off and dried, in the absence ofprecipitate the solution was extracted with AcOEt (3 30 mL).
Theorganic layer was dried (Na2SO4) and the solvent was removedunder reduced pressure.5.1.6.1.
Ethyl-[(dimethylamino)methylidene]-1-methyl-8-oxo-1,4,5,6,7,8-hexahydrocyclohepta[b]pyrrole-2-carboxylate (15b).
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