反应详情

温度

100 °C

A stirred mixture of 9-bromononanol (Aldrich)(1.0 g, 4.5 mmol), phthalimide potassium derivative (1.85 g, 10 mmol) and DMF (10 ml) was heated at 100° C. for 1 hour. The mixture was allowed to cool to room temperature and was partitioned between ethyl acetate and water. The organic layer was washed with water, brine, dried over magnesium sulfate and evaporated under reduced pressure to afford the title compound as a white solid, 1.53 g, quantitative yield. m/z (LCMS ES+, 70 v) 290.1 (MH+), 312.1 (MNa+). δH (CHCl3-d) 7.81 (2H, m), 7.73 (2H, m), 3.64 (4H, m), 1.68 (2H, m), 1.59 (2H, m), 1.32 (10H, m). Intermediate 27

1. temperatureto cool to room temperature
2. customwas partitioned between ethyl acetate and water
3. washThe organic layer was washed with water, brine
4. dry with materialdried over magnesium sulfate
5. customevaporated under reduced pressure