反应详情

Add 2 drops of DMF into 628 mg 3-iodo-4-methylbenzoic acid (2.2 mmol) in 20 mL SOCl2 and reflux for 2 h. After vacuum evaporation of SOCl2, add 6.0 mL anhydrous THF and get the pale yellow solution. Dissolve the product from step 1, 524 mg 5-(4-methyl-1H-imidazol-1-yl)-3-(trifluoromethyl)-benzenamine (2.0 mmol) in 6.0 mL anhydrous THF and add 10 mmol Et3N, and the pale yellow solution prepared previously is added drop wise till it is all added. The reaction mixture rises to room temperature for 1 hr. The reaction was quenched with addition of brine and extracted with EtOAc. The combined extraction organic layers was dried and concentrated under vacuum, the residue was purified through column chromatography to afford 873 mg desired product. (90%)

1. temperaturereflux for 2 h
2. customAfter vacuum evaporation of SOCl2
3. additionadd 6.0 mL anhydrous THF
4. customget the pale yellow solution
5. customthe pale yellow solution prepared previously
6. additionis added drop wise till it
7. customThe reaction was quenched with addition of brine
8. extractionextracted with EtOAc
9. extractionThe combined extraction organic layers
10. customwas dried
11. concentrationconcentrated under vacuum
12. customthe residue was purified through column chromatography