Hydrochloric Acid → HCID 69057401, compound

Participants

Reaction Steps

(4′-Carbamoyl-2′,2-dimethyl-biphenyl-4-ylmethyl)-(3-methyl-butyl)-carbamic acid tert-butyl ester (I-2e: 12 g, 28.3 mmol) was dissolved in ethyl acetate and treated with 20 mL of 4.0 M hydrogen chloride in dioxane. After stirring overnight at room temperature, the volatiles were removed under reduced pressure and the resulting crude material dissolved in methanol and then ethyl acetate was added to precipitate a white solid that was isolated via filtration. This solid was suspended in iso-propanol (1 g: 20 mL), heated at reflux for 20 minutes and stirred overnight at room temperature. The resulting slurry was collect via filtration, rinsing with chilled iso-propanol, and dried under vacuum to provide the title compound (E2-01).

Provenance & Evidence