反应详情

580 mg (1.44 mmol) of 4-[1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazol-4-yl]pyridine 1-oxide were suspended in a mixture of 16 ml of trifluoromethylbenzene and 4 ml of dry dichloromethane and 756 μl of tert-butylamine were added. At 0° C. 936 mg (7.2 mmol) of p-toluensulfonic anhydride were added. After 6 hours under stirring in the same conditions the solvent was removed under reduced pressure, the residue partitioned between dichloromethane and water, the organic layer dried over sodium sulphate and evaporated. The crude was then purified by flash-chromatography on a silica gel column (CH2Cl2-CH3COCH3 19/1), giving 500 mg (75%) of the title compound.

1. additionwere added
2. customAt 0° C
3. customwas removed under reduced pressure
4. customthe residue partitioned between dichloromethane and water
5. dry with materialthe organic layer dried over sodium sulphate
6. customevaporated
7. customThe crude was then purified by flash-chromatography on a silica gel column (CH2Cl2-CH3COCH3 19/1)