Hydrochloric Acid → HCID 54552857, compound

Participants

Reaction Steps

216 g of the crude product from Example 30 were dissolved in a mixture of 1.2 liters of dioxane and 800 ml of 12 percent strength sodium hydroxide solution. The solution was boiled under reflux for 15 hours and the dioxane was then stripped off and the residue was adjusted to pH 8 with 2 N hydrochloric acid. The mixture was extracted three times with ethyl acetate, the aqueous solution was adjusted to pH 3 to 4 and the product which had precipitated was filtered off. 20 g of the desired product of melting point 138° could be obtained directly by recrystallization from methanol. The mother liquor consisted of an E/Z mixture, which could not be separated by crystallization.

Provenance & Evidence