反应详情

A solution of 5'-nitro-spiro(cyclopentane-1,1'-indan)-3'-one (23.1 g; 0.1 mole) in methanol (250 ml) is hydrogenated in a shaking autoclave at about 4 atg with a Raney-nickel catalyst at 40°-60° C. The mixture is chilled, the catalyst filtered off and washed with methanol, after which the filtrate is evaporated to dryness. A light yellow powder is obtained (19.5 g; yield 97%). Said powder is dissolved in 2 N hydrochloric acid and extracted with ether, and then the aqueous phase is neutralized with 2 N sodium hydroxid solution. The precipitate is filtered off, washed with water and dried, and 18.8 g of a yellow-white crystal powder is obtained. A sample is recrystallized twice from benzene and then melts at 125° C.

1. temperatureThe mixture is chilled
2. filtrationthe catalyst filtered off
3. washwashed with methanol
4. customafter which the filtrate is evaporated to dryness
5. customA light yellow powder is obtained (19.5 g; yield 97%)
6. extractionextracted with ether
7. filtrationThe precipitate is filtered off
8. washwashed with water
9. customdried