Water → 5-Phenyl-1,3-dihydro-2H-azepin-2-one

Participants

Reaction Conditions

Reaction Steps

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.

Provenance & Evidence