HCID 53800149, compound → HCID 54427298, compound

Participants

Reaction Steps

III (11.37 g, 0.0326 mole), methanol (150 ml), and Raney nickel (2.5 g) were stirred at room temperature under 1 atmosphere of hydrogen, until one molequivalent of hydrogen had reacted. After filtration, the solvent was removed by distillation from a water bath (60°C) under reduced pressure, at last under 15 mm Hg. The residual, light yellow oil (11.4 g) was purified by preparative tlc (thin layer chromatography) on silica gel (mixture of petroleum ether (b.<50°C) and ether (2:1) as eluent). 7.25 g of the title compound were obtained as a yellowish oil. Further purification by distillation under nitrogen gave 7.05 g (62%) of the title compound as an almost colourless oil, b0.07 172°-180°C, nD25 1.4723.

Provenance & Evidence