反应详情

温度

80 °C

A mixture of Intermediate 4 (0.470 g) and 2-(oxiran-2-ylmethyl)-1H-isoindole-1,3(2H)-dione (0.410 g) was heated at 80° C. under nitrogen for 5 h. The mixture was treated with concentrated sulphuric acid (0.6 ml) then stirred at 150° C. for 42 h. The mixture was treated with water (50 ml) then washed with ethyl acetate (2×50 ml). The dark aqueous phase was basified to ˜pH 11 using 5M aqueous sodium hydroxide then extracted with ethyl acetate (2×50 ml). The combined organic extracts were washed with water and brine, dried (Na2SO4) and concentrated under vacuum to give the title compound as a brown oil (0.42 g).

1. washthen washed with ethyl acetate (2×50 ml)
2. extractionthen extracted with ethyl acetate (2×50 ml)
3. washThe combined organic extracts were washed with water and brine
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated under vacuum