反应详情

Methyl 5-benzyl-1-(2-fluorophenyl)-1H-1,2,3-triazole-4-carboxylate obtained in Step 1 as described above was dissolved in EtOH and NaOH (8.10 ml; 5 M; 40.48 mmol; 5 eq.) was added, the mixture was stirred overnight at room temperature. Water (30 mL) was added and the aqueous phase was washed with Et2O (2×30 mL). The aqueous layer was acidified to pH 2 with HCl 5 N and extracted with EtOAc (2×50 mL). The combined organics were washed with brine, dried over MgSO4 and concentrated under vacuum affording the title compound as a yellow oil. It was taken up in petroleum ether and it was sonicated. The suspension was filtered off, affording Intermediate 24 as a beige solid. 1H-NMR (DMSO-d6, 300 MHz) δ 13.43 (br s, 1H), 7.74-7.69 (m, 1H), 7.64-7.58 (m, 1H), 7.53-7.42 (m, 2H), 7.22-7.17 (m, 3H), 6.83-6.72 (m, 2H), 4.38 (s, 2H). LC/MS (Method B): 298.2 (M+H)+. HPLC (Method A) Rt 3.60 min (Purity: 92.7%).

1. washthe aqueous phase was washed with Et2O (2×30 mL)
2. extractionextracted with EtOAc (2×50 mL)
3. washThe combined organics were washed with brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated under vacuum