反应详情

温度

-78 °C

Add DIBAL in toluene (673 mL, 1.0 M, 673 mmol) to a solution of (E)-2-(4-bromo-phenyl)-3-cyclohexyl-acrylic acid (52 g, 168 mmol) in toluene (1.6 1) maintained at −78° C. Then allow the reaction mixture to slowly warm to room temperature, and stir, it for 18 h. Cool reaction mixture to 0° C. and add MeOH to destroy excess amounts of DIBAL. Add Rochelle's salt (100 mL) and HCl (2 N). Separate the layers and wash the organic layer with brine. Filter through hydrophobic filter and concentrate to obtain the title compound (48.8 g) as a white solid. MS (m/e): 277 (M+H−H2O).

1. temperatureto slowly warm to room temperature
2. temperatureCool
3. customreaction mixture to 0° C.
4. customto destroy excess amounts of DIBAL
5. customSeparate the layers
6. washwash the organic layer with brine
7. filtrationFilter
8. filtrationthrough hydrophobic filter
9. concentrationconcentrate