Isopropanol → HCID 66897681, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of ethyl 7-hydroxy-5-[4-(methylsulfonyl)phenoxy]-1H-indole-2-carboxylate (2.0 g), tributylphosphine (2.6 mL), 1,1′-(azodicarbonyl)dipiperidine (2.69 g), 2-propanol (0.81 mL) and tetrahydrofuran (50 mL) was stirred at 70° C. for 5.5 h. Furthermore, tributylphosphine (0.7 mL) and 1,1′-(azodicarbonyl)dipiperidine (0.7 g) were added to the mixture. After stirring at 70° C. for 2 h, the mixture was cooled to 0° C. and a precipitate was removed by filtration. The filtrate was concentrated and the residue was purified by basic silica gel column chromatography (ethyl acetate/hexane 1/99 to 40/60), followed by silica gel column chromatography (ethyl acetate/hexane=1/99 to 35/65, volume ratio) to give the title compound (1.87 g, 84%) as a white amorphous solid. MS 418 (MH+).

Provenance & Evidence