反応 #657312

反応方程式

2-oxopropyl methanesulfonate

3-(4-fluorophenyl)-1H-pyrazol-5-ol

potassium carbonate

→

1-{[3-(4-fluorophenyl)-1H-pyrazol-5-yl]oxy}acetone

収率 38.1%

溶媒

ethyl acetate

DMF

反応条件

後処理

1. 1
   温度the reaction mixture was heated at 60° C. for 16 h
2. 2
   洗浄washed with water (3×500 ml)
3. 3
   洗浄The organic layer was washed with brine
4. 4
   乾燥dried over sodium sulphate
5. 5
   その他evaporated under reduced pressure
6. 6
   その他to get the crude which
7. 7
   その他was then purified by column chromatography with silica gel (100-200 mesh)
8. 8
   洗浄eluted with 10-25% ethyl acetate in hexane as eluent

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]+)

出典