Hydrochloric Acid → HCID 66614124, compound

Participants

Reaction Steps

3.5 g (7.285 mmol) of the crude compound from example 55A were dissolved in ethanol (25 ml) and water (25 ml), and 174 mg (7.285 mmol) of lithium hydroxide were added. After stirring at RT for 30 min, the mixture was adjusted to pH=6 with dilute hydrochloric acid and extracted with ethyl acetate. After separation of the phases, the organic phase was washed with saturated aqueous sodium chloride solution and then dried with sodium sulfate, filtered and concentrated to dryness. The residue was slurried in acetonitrile and ethyl acetate, and insoluble constituents were filtered off. The filtrate was concentrated and the residue was purified by means of preparative HPLC (acetonitrile:water (+0.05% formic acid) gradient). 38 mg of the title compound were obtained (1% of theory).

Provenance & Evidence