反应详情

温度

100 °C

To 100 ml of 80% acetic acid in water, was added 1,2,3,4-tetrahydro-7-phenylmethoxycyclopent[b]indole-2-carboxylic acid ethyl ester (10 g, 0.03 mole). After stirring at 100° C. for four hours, the mixture was cooled, poured into 500 ml of water, stirred for five minutes, and extracted with ethyl acetate (3×). The organic layer was washed successively with water and saturated sodium chloride solution, and thereafter dried over anhydrous MgSO4. After filtering, the solution was concentrated to a dark oil (~10 g), which was eluted on a silica gel column with 5% ethyl acetate/dichloromethane via HPLC. The desired fractions were combined and concentrated to a tan solid, 1.3 g, m.p. 160°-162° C. This material was recrystallized from ether to give the product as a tan solid, 1.0 g, m.p. 161°-163° C.

1. temperaturethe mixture was cooled
2. stirringstirred for five minutes
3. extractionextracted with ethyl acetate (3×)
4. washThe organic layer was washed successively with water and saturated sodium chloride solution
5. dry with materialdried over anhydrous MgSO4
6. filtrationAfter filtering
7. concentrationthe solution was concentrated to a dark oil (~10 g), which
8. washwas eluted on a silica gel column with 5% ethyl acetate/dichloromethane via HPLC
9. concentrationconcentrated to a tan solid, 1.3 g, m.p. 160°-162° C
10. customThis material was recrystallized from ether