反应详情

A solution of 12.1 g (77 mmol) of 4-cyano-2,3-dihydro-1H-inden-1-one [see Coll. Czechoslov. Chem. Commun. 4, 3227 (1978)] in 220 ml of pyridine and 10.6 ml (77 mmol) of triethylamine is saturated with hydrogen sulfide for 3 hours at 40° and is then stirred at the same temperature for 16 hours. The reaction mixture is cooled and then concentrated to dryness by evaporation, and 300 ml of water are added to the residue. The yellow product that has crystallized out is filtered off with suction, washed with water, dried and recrystallized from ethyl acetate. In that manner there is obtained the title compound, m.p. 197° (decomp.).

1. temperatureThe reaction mixture is cooled
2. concentrationconcentrated to dryness by evaporation, and 300 ml of water
3. additionare added to the residue
4. customThe yellow product that has crystallized out
5. filtrationis filtered off with suction
6. washwashed with water
7. customdried
8. customrecrystallized from ethyl acetate