反应详情

A solution of 5-(diethoxymethyl)-3-(3-fluorophenyl)-1-methyl-1H-1,2,4-triazole (24.0 g, 86 mmol) in 4M HCl (86 mL) was stirred at 60° C. for 2 h. The mixture was concentrated in vacuo, and the residue was recrystallized from MeOH/Et2O mixture (1:1). The resulting solvate was dissolved in water/THF (1:2) and concentrated in vacuo to dryness to afford 11.33 g (47%) of the title product. Satisfactory C,H,N-analysis was obtained. 1H NMR (400 MHz, D2O+TFA): δ 4.16 (s, 3H), 6.47 (s, 1H), 7.42 (m, 1H), 7.62 (m, 1H), 7.70 (m, 1H), 7.77 (m, 1 H). LC/MS (API-ES) calcd for C10H8FN3O: 205.07, found (M+H+): 206.0; (M+18+H+): 224.0 m/z.

1. concentrationThe mixture was concentrated in vacuo
2. customthe residue was recrystallized from MeOH/Et2O mixture (1:1)
3. dissolutionThe resulting solvate was dissolved in water/THF (1:2)
4. concentrationconcentrated in vacuo to dryness