反应详情

(N-(4-cyanophenethyl)-2,2,2-trifluoroacetamide (0.61 g, 2.52 mmol) was azeotroped with benzene and was dissolved in 10 mL of anhydrous EtOH. To this solution dry HCl was bubbled though for 90 min at 0 C. The solvent was evaporated to dryness under high vacuum to give a yellow solid. This yellow solid and formohydrazide (151 mg, 2.52 mmol) was dissolved in 10 mL of dry pyridine and the resulting solution was refluxed for 2 h. After cooling to RT, pyridine was evaporated and the residue was treated with 5% HCl, extracted with EtOAc, dried over Na2SO4, filtered, and evaporated to dryness. Flash chomatography (SiO2, EtOAc/DCM=1:1 to Dcm/MeOH=10:1) afforded N-(4-(4H-1,2,4-triazol-3-yl)phenethyl)-2,2,2-trifluoroacetamide as a white solid.

1. customTo this solution dry HCl was bubbled though for 90 min at 0 C
2. customThe solvent was evaporated to dryness under high vacuum
3. customto give a yellow solid
4. temperaturethe resulting solution was refluxed for 2 h
5. custompyridine was evaporated
6. additionthe residue was treated with 5% HCl
7. extractionextracted with EtOAc
8. dry with materialdried over Na2SO4
9. filtrationfiltered
10. customevaporated to dryness