反应详情

温度

120 °C

4-bromo-1-(2-chloroethyl)-1H-pyrazole (for a preparation see Intermediate 29) (120 mg, 0.573 mmol) was mixed with potassium phthalimide (159 mg, 0.859 mmol), dissolved in N,N-Dimethylformamide (DMF) (4 mL) and stirred under nitrogen at 120° C. for 20 hours. The reaction was left to cool to room temperature and the product was partitioned between distilled water (20 mL) and EtOAc (60 mL). The aqueous layer was extracted with EtOAc (60 mL) and the organic fractions were combined, washed (brine, 30 mL), dried (MgSO4), filtered and evaporated to dryness to give a white solid. The product was purified on a 25+S Biotage silica column, eluting with cyclohexane:EtOAc (1:0 to 7:3). Product-containing fractions were evaporated to dryness to give a white solid (85 mg).

1. waitThe reaction was left
2. temperatureto cool to room temperature
3. customthe product was partitioned
4. distillationbetween distilled water (20 mL) and EtOAc (60 mL)
5. extractionThe aqueous layer was extracted with EtOAc (60 mL)
6. washwashed (brine, 30 mL)
7. dry with materialdried (MgSO4)
8. filtrationfiltered
9. customevaporated to dryness
10. customto give a white solid
11. customThe product was purified on a 25+S Biotage silica column
12. washeluting with cyclohexane:EtOAc (1:0 to 7:3)
13. customProduct-containing fractions were evaporated to dryness