反应详情

A solution of 4-iodo-1H-pyrazole-3-carboxylic acid phenylamide (670 mg; 2.14 mmol) in acetonitrile (10 ml) was treated with potassium carbonate (360 mg; 2.57 mmol)) followed by 4-methoxybenzyl chloride (320 μl; 2.35 mmol). The mixture was stirred at room temperature overnight then evaporated under reduced pressure. The residue was partitioned between ethyl acetate and brine; the ethyl acetate layer was separated, dried (MgSO4), filtered and evaporated. The crude material was purified by flash column chromatography eluting with 1:3 ethyl acetate/hexane and the product containing fractions combined and evaporated to give 660 mg of 4-iodo-1-(4-methoxy-benzyl)-1H-pyrazole-3-carboxylic acid phenylamide.

1. customthen evaporated under reduced pressure
2. customThe residue was partitioned between ethyl acetate and brine
3. customthe ethyl acetate layer was separated
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customevaporated
7. customThe crude material was purified by flash column chromatography
8. washeluting with 1:3 ethyl acetate/hexane
9. additionthe product containing fractions
10. customevaporated