Hydrochloric Acid → HCID 67076832, compound

Participants

Reaction Steps

To a solution of 1,1-dimethylethyl 4-({8-[(2-hydroxyethyl)(methyl)amino]octanoyl}amino)-benzoate (28.4 g, 72.4 mmol, e.g. which can be as prepared in Intermediate 38) in dry dichloromethane (225 ml) was added a 4M hydrogen chloride solution in 1,4-dioxane (145 ml, 579 mmol, 8 equivalents). The mixture quickly became cloudy and was stirred overnight resulting in a uniform white suspension. The solvents were evaporated off in vacuo, using a high vacuum at the end, to give the title compound (23.45 g) as a white solid. LCMS showed positive ion at m/z 336; TRET=2.01 min. NMR (d6-DMSO) appeared to show a trace of dichloromethane and 1,4-dioxane in the product.

Provenance & Evidence