反应详情

To a solution of {2-[3-(allyl-cyclopentyl-carbamoyl)-5-chloro-phenoxy]-ethyl}-pyridin-4-yl-carbamic acid tert-butyl ester (0.06 g) in tert-butanol (3.2 ml) was added a solution of potassium permanganate (0.006 g), sodium periodate (0.157 g) and sodium bicarbonate (0.051 g) in water (3.2 ml). The purple reaction mixture was stirred at room temperature for 1.5 h and then added to ethanol (25 ml) the precipitate was filtered and the filtrate evaporated in vacuo. The residue was dissolved in a mixture of dichloromethane (5 ml) and trifluoroacetic acid (5 ml) was stored at room temperature for 17 h and then concentrated under reduced pressure. The residue was subjected to preparative hplc and the title compound (0.021 g) was obtained as a colourless gum by concentration of the required fraction under reduced pressure.

1. filtrationwas filtered
2. customthe filtrate evaporated in vacuo
3. dissolutionThe residue was dissolved in a mixture of dichloromethane (5 ml) and trifluoroacetic acid (5 ml)
4. waitwas stored at room temperature for 17 h
5. concentrationconcentrated under reduced pressure