反应详情

3.00 Grams of 2,3-dihydro-4,6-dimethyl-7-hydroxy-2-phenyl-1H-inden-1-one oxime was dissolved in 55 ml of glacial acetic acid, and this solution was subjected to catalytic hydrogenation in the presence of 0.3 g of platinum oxide at room temperature under 4 atmospheric hydrogen gas pressure. The hydrogenation was terminated at the point when the stoichiometric amount of hydrogen was absorbed. The catalyst was removed by filtration and the filtrate thus obtained was concentrated. The residue thus obtained was dissolved in water and the pH of this solution was adjusted to about pH 8 by adding an aqueous solution of sodium bicarbonate, then extracted with 200 ml of chloroform. The chloroform extract was washed with water, dried with anhydrous magnesium sulfate, then concentrated under a reduced pressure. Recrystallized from ethanol to obtain 0.24 g of 1-amino-2,3-dihydro-4,6-dimethyl-7-hydroxy-2-phenyl-1H-indene Colorless needlelike crystals. Melting point: 135°-136° C.

1. customThe hydrogenation was terminated at the point when the stoichiometric amount of hydrogen
2. customwas absorbed
3. customThe catalyst was removed by filtration
4. customthe filtrate thus obtained
5. concentrationwas concentrated
6. customThe residue thus obtained
7. extractionextracted with 200 ml of chloroform
8. extractionThe chloroform extract
9. washwas washed with water
10. dry with materialdried with anhydrous magnesium sulfate
11. concentrationconcentrated under a reduced pressure
12. customRecrystallized from ethanol