反应 #657312

反应方程式

2-oxopropyl methanesulfonate

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

potassium carbonate

→

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

收率 38.1%

溶剂

ethyl acetate

DMF

反应条件

后处理

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

实验过程

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]+)

来源