Hydrochloric Acid → HCID 20592594, compound

Participants

Reaction Conditions

Reaction Steps

1.0 N NaOH (2.0 mL, 2.0 mmole) was added to a solution of ethyl (S)-10,11-dihydro-3-[3-(4-ethoxypyridin-2-ylamino)-1-propyloxy]-5H-dibenzo[a,d]cycloheptene-10-acetate (475.2 mg, 1.0 mmol) in absolute ethanol (10 mL), and the solution was warmed at 50° C. in an oil bath. After 20 hr, the reaction was concentrated and the aqueous residue was cooled to 0° C. in an ice bath. 1.0 N aqueous HCl (2.0 mL, 2.0 mmole) was slowly added with stirring. An opaque solid residue precipitated and was collected on a sintered glass funnel. Drying in a vacuum desiccator overnight gave the title compound (452.6 mg, 83%): MS (ES) m/e 447 (M+H)+. Anal. Calcd for C27H30N2O4.0.20 H2O.1.75 HCl: C, 63.10; H, 6.30; N, 5.45. Found: C, 63.10; H, 5.98; N, 5.38.

Provenance & Evidence