2-oxopropyl methanesulfonate

反応条件: temp:30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 3-(4-fluorophenyl)-1H-pyrazol-5-ol (5 g, 28 mmol) in DMF (50 ml), potassium carbonate (7.7 g, 56 mmol) was added and the mixture was stirred for 30 min at 30° C. Thereafter, 2-oxopropyl methanesulfonate (4.7 g 30 mmol) was added drop wise and the reaction mixture was heated at 60° C. for 16 h. After completion, the crude was diluted with ethyl acetate (200 ml) and washed with water (3×500 ml). The organic layer was washed with brine, dried over sodium sulphate and evaporated under reduced pressure to get the crude which was then purified by column chromatography with silica gel (100-200 mesh) eluted with 10-25% ethyl acetate in hexane as eluent to get compound 1-{[3-(4-fluorophenyl)-1H-pyrazol-5-yl]oxy}acetone (2.5 g, yield 38%). MS (ESI): 231.0 ([M+H]+) the reaction mixture was heated at 60° C. for 16 h washed with water (3×500 ml) The organic layer was washed with brine dried over sodium sulphate evaporated under reduced pressure to get the crude which was then purified by column chromatography with silica gel (100-200 mesh) eluted with 10-25% ethyl acetate in hexane as eluent

反応条件: temp:30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 3-(4-fluorophenyl)-1H-pyrazol-5-ol (5 g, 28 mmol) in DMF (50 ml), potassium carbonate (7.7 g, 56 mmol) was added and the mixture was stirred for 30 min at 30° C. Thereafter, 2-oxopropyl methanesulfonate (4.7 g 30 mmol) was added drop wise and the reaction mixture was heated at 60° C. for 16 h. After completion, the crude was diluted with ethyl acetate (200 ml) and washed with water (3×500 ml). The organic layer was washed with brine, dried over sodium sulphate and evaporated under reduced pressure to get the crude which was then purified by column chromatography with silica gel (100-200 mesh) eluted with 10-25% ethyl acetate in hexane as eluent to get compound 1-{[3-(4-fluorophenyl)-1H-pyrazol-5-yl]oxy}acetone (2.5 g, yield 38%). MS (ESI): 231.0 ([M+H]+) the reaction mixture was heated at 60° C. for 16 h washed with water (3×500 ml) The organic layer was washed with brine dried over sodium sulphate evaporated under reduced pressure to get the crude which was then purified by column chromatography with silica gel (100-200 mesh) eluted with 10-25% ethyl acetate in hexane as eluent

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

実験手順: Thirty-seven (37) mg of hydroxyacetone was dissolved in 2 ml of chloroform, and to which 0.078 ml of methanesulfonyl chloride was added. After stirring the reaction liquid at room temperature for 30 minutes, saturated aqueous sodium bicarbonate solution was added and extracted with chloroform. The extract was dried over anhydrous sodium sulfate and concentrated to provide the title compound. the reaction liquid at room temperature for 30 minutes extracted with chloroform The extract was dried over anhydrous sodium sulfate concentrated

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

実験手順: Thirty-seven (37) mg of hydroxyacetone was dissolved in 2 ml of chloroform, and to which 0.078 ml of methanesulfonyl chloride was added. After stirring the reaction liquid at room temperature for 30 minutes, saturated aqueous sodium bicarbonate solution was added and extracted with chloroform. The extract was dried over anhydrous sodium sulfate and concentrated to provide the title compound. the reaction liquid at room temperature for 30 minutes extracted with chloroform The extract was dried over anhydrous sodium sulfate concentrated

反応条件: temp:30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 3-(4-fluorophenyl)-1H-pyrazol-5-ol (5 g, 28 mmol) in DMF (50 ml), potassium carbonate (7.7 g, 56 mmol) was added and the mixture was stirred for 30 min at 30° C. Thereafter, 2-oxopropyl methanesulfonate (4.7 g 30 mmol) was added drop wise and the reaction mixture was heated at 60° C. for 16 h. After completion, the crude was diluted with ethyl acetate (200 ml) and washed with water (3×500 ml). The organic layer was washed with brine, dried over sodium sulphate and evaporated under reduced pressure to get the crude which was then purified by column chromatography with silica gel (100-200 mesh) eluted with 10-25% ethyl acetate in hexane as eluent to get compound 1-{[3-(4-fluorophenyl)-1H-pyrazol-5-yl]oxy}acetone (2.5 g, yield 38%). MS (ESI): 231.0 ([M+H]+) the reaction mixture was heated at 60° C. for 16 h washed with water (3×500 ml) The organic layer was washed with brine dried over sodium sulphate evaporated under reduced pressure to get the crude which was then purified by column chromatography with silica gel (100-200 mesh) eluted with 10-25% ethyl acetate in hexane as eluent

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

実験手順: Thirty-seven (37) mg of hydroxyacetone was dissolved in 2 ml of chloroform, and to which 0.078 ml of methanesulfonyl chloride was added. After stirring the reaction liquid at room temperature for 30 minutes, saturated aqueous sodium bicarbonate solution was added and extracted with chloroform. The extract was dried over anhydrous sodium sulfate and concentrated to provide the title compound. the reaction liquid at room temperature for 30 minutes extracted with chloroform The extract was dried over anhydrous sodium sulfate concentrated