反应详情

温度

150 °C

The 2-butoxy-5-phenyl-3H-azepine (908 g, 3.42 moles) is dissolved in 2B-3 ethanol (8172 mL) and de-ionized water (2724 mL). The solution is charged to an autoclave and heated to 150° C. for 20 hours. The solution is cooled to room temperature and concentrated under reduced pressure. Residual water is removed by azeotropic distillation from toluene (2×2 L). The residual solids are dissolved in toluene (1.7 L) and heated between 95 to 100° C. The solution is cooled to <90° C. and heptane (about 4.8 mL/g) is added. The solution is allowed to cool to room temperature, and then cooled to 0 to 5° C. using an ice bath. The solids are filtered, washed with heptane, and dried to give the title compound (559 g, 88%) as a light brown solid.

1. additionThe solution is charged to an autoclave
2. temperatureThe solution is cooled to room temperature
3. concentrationconcentrated under reduced pressure
4. customResidual water is removed by azeotropic distillation from toluene (2×2 L)
5. dissolutionThe residual solids are dissolved in toluene (1.7 L)
6. temperatureheated between 95 to 100° C
7. temperatureThe solution is cooled to <90° C.
8. additionheptane (about 4.8 mL/g) is added
9. temperatureto cool to room temperature
10. temperaturecooled to 0 to 5° C.
11. filtrationThe solids are filtered
12. washwashed with heptane
13. customdried