反应详情

温度

150 °C

To a solution of 2-benzyl-9a-(2-fluoroethyl)-8,9,9a,10-tetrahydroindeno[2,1-e]indazol-7(2H)-one (1.0 g, 2.5 mmol) in 25 mL, of dimethylformamide was added lithium chloride (1.05 g, 25 mmol) and the stirred mixture was heated to 150° C. After heating for 89 hours, the reaction mixture was cooled to room temperature and partitioned between EtOAc and water. The organic phase was washed thoroughly with water (3×) followed by brine and dried over MgSO4. The solution was concentrated under vacuum and the residue chromatographed on silica gel (elution with 15:85 to 75:25 EtOAc/hexanes) to yield 2-benzyl-2,9,10,11-tetrahydro-8,10a-methanoazuleno[2,1-e]indazol-7(8H)-one as a solid.

1. temperatureAfter heating for 89 hours
2. temperaturethe reaction mixture was cooled to room temperature
3. custompartitioned between EtOAc and water
4. washThe organic phase was washed thoroughly with water (3×)
5. dry with materialdried over MgSO4
6. concentrationThe solution was concentrated under vacuum
7. customthe residue chromatographed on silica gel (elution with 15:85 to 75:25 EtOAc/hexanes)