反应详情

4-methyl-6-[3-(trifluoromethyl)phenoxy] picolinic acid hydrazide (0.38 g, 0.0012 mol) was dissolved in 5 ml of acetic acid. The obtained solution was mixed with 2,2,3,3,3-pentafluoropropionaldehyde monohydrate (0.40 g, 0.0012×2 mol), and then the resultant mixture was stirred at 80° C. for 3 hours. Thereafter, a chilled water was poured into the obtained reaction solution which was then distributed in ethyl acetate-water. The organic phase separated from the solution was washed with water and then dried with anhydrous sodium sulfate. After distilling off the solvent from the dried product, the obtained distillation residues were purified by silica gel column chromatography (eluting solution: ethyl acetate/hexane), thereby obtaining an aimed product.

1. customThe organic phase separated from the solution
2. washwas washed with water
3. dry with materialdried with anhydrous sodium sulfate
4. distillationAfter distilling off the solvent from the dried product
5. distillationthe obtained distillation residues
6. customwere purified by silica gel column chromatography (eluting solution: ethyl acetate/hexane)