(E)-1-cyclopropyl-3-(dimethylamino)prop-2-en-1-one

反応条件: temp:150.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: (2E)-1-cyclopropyl-3-(dimethylamino)prop-2-en-1-one (327 mg, 2.35 mmol) and phenylhydrazine (0.35 ml, 3.5 mmol) were added to ethanol (5 ml). The reaction mixture was heated to 150° C. in the Biotage Initiator Series microwave reactor. After 30 minutes, the reaction mixture was cooled and concentrated. The residue was purified by column chromatography on silica gel (ethyl acetate/hexanes gradient) to afford 3-cyclopropyl-1-phenyl-1H-pyrazole (faster eluting isomer) and 5-cyclopropyl-1-phenyl-1H-pyrazole (slower eluting isomer). the reaction mixture was cooled concentrated The residue was purified by column chromatography on silica gel (ethyl acetate/hexanes gradient)

反応条件: temp:150.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To N,N-dimethylformamide dimethyl acetal (9.51 ml, 71.3 mmol) was added cyclopropyl methyl ketone (3.34 ml, 35.7 mmol) and the mixture was heated to 150° C. in a sealed vessel. After 16 hours, the reaction mixture was cooled and concentrated to afford (2E)-1-cyclopropyl-3-(dimethylamino)prop-2-en-1-one which was used without further purification. the reaction mixture was cooled concentrated