反应详情

温度

100 °C

A mixture of 14.7 g 5-[5-(2,6-dichloro-4-cyanophenoxy)pentyl]-3-methylisoxazole (Example 32a), 2.96 g sodium azide and 0.32 g ammonium chloride in 150 ml dimethylformamide was stirred and heated at 100° C. for 24 hrs. The reaction mixture was concentrated in vacuo, and the residue was dissolved in ethyl acetate and washed with 2N hydrochloric acid. The organic layer was dried over magnesium sulfate and concentrated in vacuo to a solid residue. The latter was recrystallized from ethyl acetate to give 10.3 g (62%) 5-{5-[2,6-dichloro-4-(1H-tetrazol-5yl)phenoxy]pentyl}-3-methylisoxazole, m.p. 122-123° C.

1. concentrationThe reaction mixture was concentrated in vacuo
2. dissolutionthe residue was dissolved in ethyl acetate
3. washwashed with 2N hydrochloric acid
4. dry with materialThe organic layer was dried over magnesium sulfate
5. concentrationconcentrated in vacuo to a solid residue
6. customThe latter was recrystallized from ethyl acetate