تفاعل #657312

معادلة التفاعل

2-oxopropyl methanesulfonate

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

potassium carbonate

→

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

المردود 38.1%

المذيبات

ethyl acetate

DMF

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe reaction mixture was heated at 60° C. for 16 h
2. 2
   غسيلwashed with water (3×500 ml)
3. 3
   غسيلThe organic layer was washed with brine
4. 4
   تجفيفdried over sodium sulphate
5. 5
   أخرىevaporated under reduced pressure
6. 6
   أخرىto get the crude which
7. 7
   أخرىwas then purified by column chromatography with silica gel (100-200 mesh)
8. 8
   غسيلeluted with 10-25% ethyl acetate in hexane as eluent

الإجراء التجريبي

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]+)

المصدر