反应详情

温度

25 °C

To a clear solution of 3-benzyl-3-[(1,2,4-triazol-1-yl)methyl]-2(3H)-benzofuranone (11 g, 0.0360 mole) and methanol (100 mL), potassium hydroxide (45% solution) (0.5 g, 0.0750 mole) was added and the reaction mixture heated with stirring at reflux for 3 hours. The reaction mixture was then cooled to 25° C. and iodomethane (6.1 g, 0.0750 mole) added and the reaction mixture continued to stir at 50° C. for an additional 3 hours. The reaction solvent was then removed by distillation, and the residue stirred with hydrochloric acid (5 g, 0.37 mole) and 100 mL of water. The precipitated solid was filtered by suction and washed by 100 mL of hot ethyl acetate. The remaining solid was dried and gave 7.0 g, melting point 250°-252° C. (yield 57%), Example 95 of Table 1.

1. temperaturethe reaction mixture heated
2. temperatureat reflux for 3 hours
3. stirringto stir at 50° C. for an additional 3 hours
4. customThe reaction solvent was then removed by distillation
5. filtrationThe precipitated solid was filtered by suction
6. washwashed by 100 mL of hot ethyl acetate
7. customThe remaining solid was dried
8. customgave 7.0 g, melting point 250°-252° C. (yield 57%), Example 95 of Table 1