反应详情

To a solution of (3-{3′-[(2,3-dihydro-1H-inden-2-ylamino)methyl]-4-biphenylyl}-1H-1,2,4-triazol-1-yl)methyl 2,2-dimethylpropanoate (0.084 g, 0.17 mmol, Example X-3) in EtOH (1.5 mL) was added a 4.37 M solution of NaOMe in MeOH (0.08 mL, 0.35 mmol). The mixture was stirred for 50 min at RT. A 1.2M solution of concentrated HCl in EtOH was added (1.2 mL), and the mixture was heated at 80° C. for 1 h. The reaction mixture was cooled, diluted with water, and basified to a pH of 10 with addition of saturated Na2CO3 (aq). The mixture was extracted with EtOAc. The combined organic extracts were washed with water and brine, dried with anhydrous Na2SO4, and concentrated in vacuo. The residue was dissolved in CH2Cl2 and MeOH, and 4N HCl in dioxane was added (0.2 mL). After stirring for 15 min, the precipitate was filtered, washed with CH2Cl2, and dried, affording the title compound as a colorless solid (0.057 g, 89%). (M+H) 367, 1.74 min (LC/MS Method B).

1. temperaturethe mixture was heated at 80° C. for 1 h
2. temperatureThe reaction mixture was cooled
3. extractionThe mixture was extracted with EtOAc
4. washThe combined organic extracts were washed with water and brine
5. dry with materialdried with anhydrous Na2SO4
6. concentrationconcentrated in vacuo
7. dissolutionThe residue was dissolved in CH2Cl2
8. additionMeOH, and 4N HCl in dioxane was added (0.2 mL)
9. stirringAfter stirring for 15 min
10. filtrationthe precipitate was filtered
11. washwashed with CH2Cl2
12. customdried