反应详情

A THF solution of 1 g (7.3 mmol) of anthranilic acid was dropped into a mixed solution under reflux of 0.77 ml (8.0 mmol) of 1,3-cyclohexadiene, 1.1 ml of isoamyl nitrite and 50 ml of tetrahydrofuran. Then, the resultant solution was heated and refluxed for 2 hours to remove THF, extracted with chloroform, washed with distilled water and saturated saline, dried with anhydrous sodium sulfate and purified with silica gel column-chromatography-(chloroform) to obtain 1,4-dihydro-1,4-ethanonaphthalene (0.89 g, 5.7 mmol, yield: 78%).

1. temperaturerefluxed for 2 hours
2. customto remove THF
3. extractionextracted with chloroform
4. washwashed with distilled water and saturated saline
5. dry with materialdried with anhydrous sodium sulfate
6. custompurified with silica gel column-chromatography-(chloroform)