Hydrochloric Acid → HCID 44139914, compound

Participants

Reaction Steps

10.0 g (38.0 mmol) of the compound from Example 12 are initially charged in 300 ml of acetic acid. 20 ml of a 4 N solution of hydrogen chloride in dioxane and 5.0 g (4.7 mmol) of palladium on carbon (10%) are added and the mixture is hydrogenated at RT under atmospheric pressure for 96 h. Water is then added until the organic solid formed has gone back into solution, and the catalyst is filtered off through silica gel. The filtrate is concentrated and the residue is purified by column chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate mixture). The product obtained is then stirred in a 4 N solution of hydrogen chloride in dioxane for 30 min, and the solid is filtered off and dried under high vacuum. The solid is then dissolved in about 300 ml of water, and the solution is lyophilized.

Provenance & Evidence