Potassium Hydroxide → HCID 178419868, compound

Participants

Reaction Conditions

Reaction Steps

9a-(1H-Imidazol-4-yl)-1,2,3,4,4a,9a-hexahydrofluoren-9-one (2.5 g) was mixed with di(ethylene glycol) (50 ml), hydrazine hydrate (7.2 ml) and KOH (9.5 g). The mixture was heated at 150° C. for 30 minutes and at 190° C. for 4 hours. After cooling to the ambient temperature the reaction mixture was diluted with water (150 ml) and extracted with CH2Cl2 (4×50 ml). The organic phase was washed with water (30 ml). The organic phase was mixed with water (200 ml) and the pH was adjusted to 1 with concentrated HCl solution. The layers were separated and the aqueous phase was washed with CH2Cl2 (2×30 ml). The aqueous phase was mixed with CH2Cl2 (150 ml) and the pH was adjusted to 11.5-13.5 with 48% NaOH solution. The phases were separated and the aqueous phase was extracted with CH2Cl2 (2×30 ml). The combined organic phases were washed with water (50 ml), dried over Na2SO4 and evaporated. The yield was 1.4 g.

Provenance & Evidence